Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email N.LONG@IC.AC.UK _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _publ_contact_author_name 'Dr Nicholas Long' _publ_contact_author_address ; Department of Chemistry Imperial College, London Exhibition Road South Kensington London SW7 2AY UNITED KINGDOM ; _publ_section_title ; Synthesis, spectroscopic and olefin polymerisation studies on nickel and palladium complexes containing ferrocene substituted nitrogen donor ligands ; loop_ _publ_author_name N.Long V.C.Gibson C.Halliwell P.J.Oxford A.M.Smith A.J.P.White D.J.Williams data_Compound_5B _database_code_CSD 196185 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24.50 H23.50 N4 Cl5.50 Fe Pd2' _chemical_formula_weight 837.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8522(11) _cell_length_b 7.6614(13) _cell_length_c 19.6254(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.844(6) _cell_angle_gamma 90.00 _cell_volume 2828.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 11.18 _cell_measurement_theta_max 22.49 _exptl_crystal_description prisms _exptl_crystal_colour 'Deep orange/red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method ? _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 19.182 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2399 _exptl_absorpt_correction_T_max 0.6998 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4350 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 60.00 _reflns_number_total 4206 _reflns_number_observed 3291 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 256 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.2036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3950 _refine_ls_number_parameters 373 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_obs 0.0494 _refine_ls_wR_factor_all 0.1262 _refine_ls_wR_factor_obs 0.1132 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.39298(5) 0.2056(2) 0.33197(6) 0.0263(3) Uani 1 d . . Pd1 Pd 0.29826(3) 0.27358(8) 0.53883(3) 0.0286(2) Uani 1 d . . Pd2 Pd 0.23315(3) 0.59042(8) 0.40134(3) 0.0367(2) Uani 1 d D . Cl1 Cl 0.42087(10) 0.2910(3) 0.54927(12) 0.0488(5) Uani 1 d . . Cl2 Cl 0.19109(12) 0.4387(4) 0.30566(14) 0.0615(7) Uani 1 d . . C1 C 0.2985(5) 0.3951(12) 0.6323(4) 0.036(2) Uani 1 d . . H1A H 0.3459(8) 0.4320(74) 0.6463(15) 0.054 Uiso 1 calc R . H1B H 0.2820(32) 0.3151(28) 0.6654(8) 0.054 Uiso 1 calc R . H1C H 0.2677(27) 0.4949(49) 0.6289(9) 0.054 Uiso 1 calc R . C2 C 0.1281(5) 0.6489(42) 0.4128(16) 0.027(3) Uani 0.50 d PDU 1 H2A H 0.1160(18) 0.6165(151) 0.4579(26) 0.040 Uiso 0.50 calc PR 1 H2B H 0.0986(6) 0.5857(121) 0.3796(42) 0.040 Uiso 0.50 calc PR 1 H2C H 0.1206(14) 0.7720(46) 0.4064(62) 0.040 Uiso 0.50 calc PR 1 Cl3' Cl 0.1185(2) 0.6721(15) 0.4180(6) 0.068(2) Uani 0.50 d PDU 2 C3 C 0.3277(4) 0.0751(10) 0.3938(4) 0.0244(15) Uani 1 d . . C4 C 0.3116(4) 0.0251(12) 0.3232(4) 0.036(2) Uani 1 d . . H4A H 0.2678(4) 0.0365(12) 0.2988(4) 0.043 Uiso 1 calc R . C5 C 0.3733(5) -0.0431(12) 0.2986(4) 0.042(2) Uani 1 d . . H5A H 0.3783(5) -0.0830(12) 0.2544(4) 0.050 Uiso 1 calc R . C6 C 0.4283(5) -0.0413(14) 0.3535(5) 0.048(2) Uani 1 d . . H6A H 0.4745(5) -0.0822(14) 0.3511(5) 0.057 Uiso 1 calc R . C7 C 0.4002(4) 0.0321(12) 0.4102(4) 0.036(2) Uani 1 d . . H7A H 0.4248(4) 0.0504(12) 0.4523(4) 0.043 Uiso 1 calc R . C8 C 0.3849(4) 0.4691(12) 0.3468(4) 0.035(2) Uani 1 d . . C9 C 0.4574(4) 0.4124(12) 0.3583(5) 0.038(2) Uani 1 d . . H9A H 0.4858(4) 0.4235(12) 0.3987(5) 0.045 Uiso 1 calc R . C10 C 0.4772(4) 0.3374(15) 0.2974(5) 0.048(2) Uani 1 d . . H10A H 0.5217(4) 0.2912(15) 0.2904(5) 0.057 Uiso 1 calc R . C11 C 0.4187(5) 0.3430(14) 0.2481(4) 0.044(2) Uani 1 d . . H11A H 0.4182(5) 0.3002(14) 0.2038(4) 0.053 Uiso 1 calc R . C12 C 0.3620(4) 0.4239(12) 0.2779(4) 0.037(2) Uani 1 d . . H12A H 0.3172(4) 0.4449(12) 0.2567(4) 0.045 Uiso 1 calc R . N13 N 0.2807(3) 0.1428(8) 0.4401(3) 0.0237(12) Uani 1 d . . C13 C 0.2140(4) 0.1261(11) 0.4241(4) 0.032(2) Uani 1 d . . H13A H 0.1986(4) 0.0735(11) 0.3830(4) 0.038 Uiso 1 calc R . C14 C 0.1626(4) 0.1892(12) 0.4700(4) 0.036(2) Uani 1 d . . N15 N 0.1891(4) 0.2612(9) 0.5293(3) 0.035(2) Uani 1 d . . C16 C 0.1423(6) 0.3158(17) 0.5722(6) 0.060(3) Uani 1 d . . H16A H 0.1600(6) 0.3637(17) 0.6134(6) 0.072 Uiso 1 calc R . C17 C 0.0715(5) 0.3074(20) 0.5609(7) 0.075(4) Uani 1 d . . H17A H 0.0414(5) 0.3519(20) 0.5923(7) 0.090 Uiso 1 calc R . C18 C 0.0444(5) 0.2293(20) 0.5002(7) 0.073(4) Uani 1 d . . H18A H -0.0044(5) 0.2165(20) 0.4912(7) 0.087 Uiso 1 calc R . C19 C 0.0907(5) 0.1724(16) 0.4546(5) 0.050(2) Uani 1 d . . H19A H 0.0738(5) 0.1227(16) 0.4135(5) 0.060 Uiso 1 calc R . N20 N 0.3444(3) 0.5563(8) 0.3947(3) 0.0288(14) Uani 1 d . . C20 C 0.3799(5) 0.6278(12) 0.4447(4) 0.039(2) Uani 1 d . . H20A H 0.4293(5) 0.6253(12) 0.4469(4) 0.047 Uiso 1 calc R . C21 C 0.3431(4) 0.7135(10) 0.4982(4) 0.035(2) Uani 1 d . . N22 N 0.2711(4) 0.7125(9) 0.4895(4) 0.038(2) Uani 1 d . . C23 C 0.2337(6) 0.7862(15) 0.5395(6) 0.060(3) Uani 1 d . . H23A H 0.1843(6) 0.7840(15) 0.5351(6) 0.071 Uiso 1 calc R . C24 C 0.2672(7) 0.8631(14) 0.5958(6) 0.061(3) Uani 1 d . . H24A H 0.2406(7) 0.9126(14) 0.6291(6) 0.074 Uiso 1 calc R . C25 C 0.3398(7) 0.8670(15) 0.6032(6) 0.063(3) Uani 1 d . . H25A H 0.3627(7) 0.9200(15) 0.6412(6) 0.076 Uiso 1 calc R . C26 C 0.3793(6) 0.7913(14) 0.5535(5) 0.052(2) Uani 1 d . . H26A H 0.4287(6) 0.7932(14) 0.5576(5) 0.063 Uiso 1 calc R . C30 C 0.0788(6) 0.7481(22) 0.2266(7) 0.079(4) Uani 1 d . . H30A H 0.0933(6) 0.6719(22) 0.2652(7) 0.095 Uiso 0.50 calc PR 1 H30B H 0.0900(6) 0.6573(22) 0.2593(7) 0.095 Uiso 0.50 d PR 2 Cl31 Cl -0.0080(9) 0.8060(30) 0.2425(13) 0.141(9) Uani 0.50 d P 1 Cl32 Cl 0.0830(5) 0.5973(16) 0.1492(7) 0.085(3) Uani 0.50 d P 1 Cl33 Cl 0.1423(11) 0.8837(19) 0.2256(10) 0.133(7) Uani 0.50 d P 1 Cl34 Cl -0.0098(9) 0.8157(25) 0.2219(11) 0.117(7) Uani 0.50 d P 2 Cl35 Cl 0.0875(10) 0.6938(24) 0.1485(9) 0.140(7) Uani 0.50 d P 2 Cl36 Cl 0.1294(6) 0.9601(20) 0.2432(7) 0.104(4) Uani 0.50 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0212(5) 0.0386(7) 0.0203(6) 0.0049(5) 0.0088(4) 0.0009(5) Pd1 0.0315(3) 0.0303(3) 0.0239(3) 0.0026(2) 0.0020(2) -0.0011(2) Pd2 0.0342(3) 0.0317(3) 0.0440(4) 0.0060(3) 0.0008(2) 0.0035(2) Cl1 0.0327(9) 0.0627(14) 0.0495(12) 0.0018(11) -0.0076(8) -0.0108(10) Cl2 0.0463(11) 0.070(2) 0.0654(15) -0.0119(13) -0.0142(11) 0.0068(12) C1 0.051(4) 0.035(4) 0.022(4) -0.011(3) -0.003(3) 0.004(4) C2 0.026(3) 0.027(3) 0.027(3) -0.0005(10) 0.0025(11) 0.0010(10) Cl3' 0.036(2) 0.087(5) 0.083(4) -0.011(4) 0.013(3) 0.013(3) C3 0.032(3) 0.022(4) 0.021(3) 0.004(3) 0.011(3) -0.003(3) C4 0.032(4) 0.045(5) 0.031(4) -0.005(4) 0.006(3) -0.010(4) C5 0.053(5) 0.040(5) 0.034(4) 0.004(4) 0.016(4) 0.000(4) C6 0.044(4) 0.051(6) 0.052(5) 0.005(5) 0.031(4) 0.023(4) C7 0.030(3) 0.045(5) 0.035(4) 0.011(4) 0.010(3) 0.006(4) C8 0.034(4) 0.044(5) 0.027(4) 0.010(4) -0.003(3) -0.009(4) C9 0.024(3) 0.045(5) 0.045(5) -0.005(4) 0.008(3) -0.004(4) C10 0.037(4) 0.068(7) 0.041(5) 0.005(5) 0.027(4) -0.019(5) C11 0.057(5) 0.053(6) 0.024(4) 0.004(4) 0.012(4) -0.012(5) C12 0.038(4) 0.050(5) 0.025(4) 0.013(4) 0.002(3) -0.011(4) N13 0.024(3) 0.027(3) 0.020(3) 0.007(3) 0.002(2) -0.002(2) C13 0.020(3) 0.040(5) 0.035(4) 0.006(4) 0.009(3) -0.001(3) C14 0.030(4) 0.041(5) 0.039(4) 0.004(4) 0.010(3) 0.001(4) N15 0.042(4) 0.034(4) 0.031(4) -0.002(3) 0.015(3) 0.004(3) C16 0.056(6) 0.079(8) 0.047(6) -0.013(6) 0.024(5) 0.004(6) C17 0.041(5) 0.103(10) 0.086(9) -0.028(8) 0.040(5) 0.001(6) C18 0.028(4) 0.105(11) 0.087(9) 0.000(8) 0.021(5) 0.000(5) C19 0.034(4) 0.071(7) 0.046(5) -0.004(5) 0.013(4) 0.000(4) N20 0.034(3) 0.022(3) 0.031(3) 0.010(3) 0.007(3) -0.004(3) C20 0.044(4) 0.035(5) 0.039(5) 0.006(4) 0.003(4) -0.010(4) C21 0.045(4) 0.020(4) 0.039(4) 0.007(3) 0.006(3) -0.002(3) N22 0.054(4) 0.024(3) 0.037(4) 0.010(3) 0.012(3) 0.006(3) C23 0.067(6) 0.050(6) 0.064(7) 0.013(5) 0.022(5) 0.017(5) C24 0.099(8) 0.036(5) 0.051(6) -0.003(5) 0.019(6) 0.011(6) C25 0.095(8) 0.046(6) 0.049(6) 0.005(5) 0.000(6) -0.003(6) C26 0.070(6) 0.045(6) 0.042(5) -0.004(4) 0.006(5) -0.006(5) C30 0.054(6) 0.113(12) 0.072(8) 0.035(8) 0.008(6) 0.008(7) Cl31 0.082(10) 0.100(11) 0.251(21) 0.047(12) 0.077(12) 0.017(7) Cl32 0.064(4) 0.121(8) 0.069(5) -0.009(6) 0.000(3) 0.009(5) Cl33 0.174(14) 0.088(9) 0.132(12) 0.026(7) -0.022(9) -0.063(9) Cl34 0.080(9) 0.092(11) 0.174(13) -0.053(10) -0.034(8) 0.022(7) Cl35 0.156(11) 0.185(17) 0.079(7) -0.023(11) 0.015(7) 0.011(12) Cl36 0.073(4) 0.132(12) 0.101(7) 0.039(8) -0.026(5) -0.058(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C7 2.028(8) . ? Fe C10 2.036(8) . ? Fe C11 2.039(9) . ? Fe C6 2.040(10) . ? Fe C5 2.041(10) . ? Fe C9 2.042(9) . ? Fe C12 2.045(9) . ? Fe C3 2.046(7) . ? Fe C8 2.047(10) . ? Fe C4 2.064(8) . ? Pd1 N15 2.056(7) . ? Pd1 C1 2.057(7) . ? Pd1 N13 2.187(6) . ? Pd1 Cl1 2.311(2) . ? Pd2 N22 2.052(8) . ? Pd2 C2 2.058(2) . ? Pd2 N20 2.127(6) . ? Pd2 Cl3' 2.294(2) . ? Pd2 Cl2 2.303(3) . ? C3 N13 1.410(10) . ? C3 C7 1.421(11) . ? C3 C4 1.451(11) . ? C4 C5 1.392(12) . ? C5 C6 1.444(14) . ? C6 C7 1.384(13) . ? C8 N20 1.417(11) . ? C8 C12 1.434(11) . ? C8 C9 1.437(11) . ? C9 C10 1.398(13) . ? C10 C11 1.418(13) . ? C11 C12 1.397(13) . ? N13 C13 1.281(9) . ? C13 C14 1.450(11) . ? C14 N15 1.352(11) . ? C14 C19 1.375(12) . ? N15 C16 1.328(12) . ? C16 C17 1.34(2) . ? C17 C18 1.40(2) . ? C18 C19 1.363(15) . ? N20 C20 1.274(11) . ? C20 C21 1.454(13) . ? C21 N22 1.356(11) . ? C21 C26 1.378(13) . ? N22 C23 1.368(13) . ? C23 C24 1.37(2) . ? C24 C25 1.37(2) . ? C25 C26 1.39(2) . ? C30 Cl33 1.59(2) . ? C30 Cl35 1.61(2) . ? C30 Cl31 1.74(2) . ? C30 Cl34 1.75(2) . ? C30 Cl36 1.90(2) . ? C30 Cl32 1.91(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Fe C10 124.3(4) . . ? C7 Fe C11 160.3(4) . . ? C10 Fe C11 40.7(4) . . ? C7 Fe C6 39.8(4) . . ? C10 Fe C6 106.1(4) . . ? C11 Fe C6 123.6(4) . . ? C7 Fe C5 68.5(4) . . ? C10 Fe C5 119.0(4) . . ? C11 Fe C5 105.7(4) . . ? C6 Fe C5 41.4(4) . . ? C7 Fe C9 108.0(4) . . ? C10 Fe C9 40.1(4) . . ? C11 Fe C9 68.5(4) . . ? C6 Fe C9 119.1(4) . . ? C5 Fe C9 153.9(3) . . ? C7 Fe C12 158.6(3) . . ? C10 Fe C12 67.9(4) . . ? C11 Fe C12 40.0(4) . . ? C6 Fe C12 160.7(4) . . ? C5 Fe C12 123.9(4) . . ? C9 Fe C12 68.9(3) . . ? C7 Fe C3 40.8(3) . . ? C10 Fe C3 162.4(3) . . ? C11 Fe C3 156.4(3) . . ? C6 Fe C3 68.0(3) . . ? C5 Fe C3 68.4(3) . . ? C9 Fe C3 126.9(3) . . ? C12 Fe C3 123.1(3) . . ? C7 Fe C8 122.7(3) . . ? C10 Fe C8 68.0(4) . . ? C11 Fe C8 68.2(4) . . ? C6 Fe C8 155.7(4) . . ? C5 Fe C8 162.4(3) . . ? C9 Fe C8 41.1(3) . . ? C12 Fe C8 41.0(3) . . ? C3 Fe C8 110.1(3) . . ? C7 Fe C4 68.6(3) . . ? C10 Fe C4 153.7(4) . . ? C11 Fe C4 119.6(3) . . ? C6 Fe C4 68.1(4) . . ? C5 Fe C4 39.6(3) . . ? C9 Fe C4 165.3(3) . . ? C12 Fe C4 108.7(3) . . ? C3 Fe C4 41.3(3) . . ? C8 Fe C4 127.7(3) . . ? N15 Pd1 C1 92.5(3) . . ? N15 Pd1 N13 78.9(2) . . ? C1 Pd1 N13 171.4(3) . . ? N15 Pd1 Cl1 179.3(2) . . ? C1 Pd1 Cl1 87.3(2) . . ? N13 Pd1 Cl1 101.3(2) . . ? N22 Pd2 C2 95.3(9) . . ? N22 Pd2 N20 79.5(3) . . ? C2 Pd2 N20 173.8(9) . . ? N22 Pd2 Cl3' 92.0(4) . . ? N20 Pd2 Cl3' 170.0(3) . . ? N22 Pd2 Cl2 176.8(2) . . ? C2 Pd2 Cl2 85.3(9) . . ? N20 Pd2 Cl2 100.1(2) . . ? Cl3' Pd2 Cl2 88.7(3) . . ? N13 C3 C7 125.2(7) . . ? N13 C3 C4 127.7(6) . . ? C7 C3 C4 107.0(7) . . ? N13 C3 Fe 129.2(5) . . ? C7 C3 Fe 68.9(4) . . ? C4 C3 Fe 70.0(4) . . ? C5 C4 C3 107.7(7) . . ? C5 C4 Fe 69.3(5) . . ? C3 C4 Fe 68.7(4) . . ? C4 C5 C6 108.2(7) . . ? C4 C5 Fe 71.1(5) . . ? C6 C5 Fe 69.2(6) . . ? C7 C6 C5 108.0(7) . . ? C7 C6 Fe 69.7(5) . . ? C5 C6 Fe 69.3(5) . . ? C6 C7 C3 109.1(8) . . ? C6 C7 Fe 70.5(5) . . ? C3 C7 Fe 70.3(4) . . ? N20 C8 C12 126.7(7) . . ? N20 C8 C9 126.0(7) . . ? C12 C8 C9 107.3(8) . . ? N20 C8 Fe 127.4(6) . . ? C12 C8 Fe 69.4(5) . . ? C9 C8 Fe 69.2(5) . . ? C10 C9 C8 107.2(8) . . ? C10 C9 Fe 69.7(5) . . ? C8 C9 Fe 69.6(5) . . ? C9 C10 C11 109.3(8) . . ? C9 C10 Fe 70.2(5) . . ? C11 C10 Fe 69.8(5) . . ? C12 C11 C10 108.1(8) . . ? C12 C11 Fe 70.2(5) . . ? C10 C11 Fe 69.5(5) . . ? C11 C12 C8 108.1(7) . . ? C11 C12 Fe 69.8(5) . . ? C8 C12 Fe 69.6(5) . . ? C13 N13 C3 117.0(6) . . ? C13 N13 Pd1 110.6(5) . . ? C3 N13 Pd1 132.4(4) . . ? N13 C13 C14 119.9(7) . . ? N15 C14 C19 121.9(8) . . ? N15 C14 C13 116.6(7) . . ? C19 C14 C13 121.5(8) . . ? C16 N15 C14 116.8(8) . . ? C16 N15 Pd1 129.2(7) . . ? C14 N15 Pd1 114.0(5) . . ? N15 C16 C17 125.2(11) . . ? C16 C17 C18 117.7(10) . . ? C19 C18 C17 118.8(9) . . ? C18 C19 C14 119.4(10) . . ? C20 N20 C8 115.8(7) . . ? C20 N20 Pd2 111.6(6) . . ? C8 N20 Pd2 132.6(5) . . ? N20 C20 C21 120.1(8) . . ? N22 C21 C26 122.7(9) . . ? N22 C21 C20 115.3(8) . . ? C26 C21 C20 122.0(8) . . ? C21 N22 C23 117.8(9) . . ? C21 N22 Pd2 113.5(6) . . ? C23 N22 Pd2 128.7(7) . . ? N22 C23 C24 121.7(11) . . ? C25 C24 C23 119.9(11) . . ? C24 C25 C26 119.7(11) . . ? C21 C26 C25 118.2(10) . . ? Cl33 C30 Cl31 123.6(14) . . ? Cl35 C30 Cl34 100.6(12) . . ? Cl35 C30 Cl36 107.6(11) . . ? Cl34 C30 Cl36 102.9(11) . . ? Cl33 C30 Cl32 108.3(10) . . ? Cl31 C30 Cl32 112.6(11) . . ? _refine_diff_density_max 0.921 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.131 data_Compound_1A _database_code_CSD 196186 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H18 N4 Fe' _chemical_formula_weight 394.25 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.4177(14) _cell_length_b 10.4738(14) _cell_length_c 20.9191(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3597.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.85 _cell_measurement_theta_max 12.52 _exptl_crystal_description blocks _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method ? _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.78 _diffrn_reflns_number 3148 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3148 _reflns_number_observed 2175 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 308 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2840 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_obs 0.0406 _refine_ls_wR_factor_all 0.1108 _refine_ls_wR_factor_obs 0.0827 _refine_ls_goodness_of_fit_all 1.019 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.189 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.86716(2) 0.17684(4) 0.60254(2) 0.03548(13) Uani 1 d . . C1 C 0.9898(2) 0.1447(3) 0.6139(2) 0.0400(7) Uani 1 d . . C2 C 0.9439(2) 0.0612(3) 0.6533(2) 0.0459(8) Uani 1 d . . H2A H 0.9468(2) 0.0563(3) 0.6976(2) 0.055 Uiso 1 calc R . C3 C 0.8926(2) -0.0137(3) 0.6135(2) 0.0542(9) Uani 1 d . . H3A H 0.8568(2) -0.0769(3) 0.6271(2) 0.065 Uiso 1 calc R . C4 C 0.9058(2) 0.0245(4) 0.5500(2) 0.0561(10) Uani 1 d . . H4A H 0.8799(2) -0.0093(4) 0.5143(2) 0.067 Uiso 1 calc R . C5 C 0.9653(2) 0.1237(4) 0.5493(2) 0.0489(8) Uani 1 d . . H5A H 0.9845(2) 0.1667(4) 0.5135(2) 0.059 Uiso 1 calc R . C6 C 0.8413(2) 0.3652(3) 0.6218(2) 0.0385(7) Uani 1 d . . C7 C 0.7969(2) 0.2823(3) 0.6643(2) 0.0421(8) Uani 1 d . . H7A H 0.8001(2) 0.2819(3) 0.7087(2) 0.051 Uiso 1 calc R . C8 C 0.7475(2) 0.2016(3) 0.6264(2) 0.0499(8) Uani 1 d . . H8A H 0.7125(2) 0.1388(3) 0.6417(2) 0.060 Uiso 1 calc R . C9 C 0.7604(2) 0.2328(4) 0.5612(2) 0.0535(9) Uani 1 d . . H9A H 0.7351(2) 0.1942(4) 0.5265(2) 0.064 Uiso 1 calc R . C10 C 0.8186(2) 0.3327(4) 0.5580(2) 0.0471(8) Uani 1 d . . H10A H 0.8384(2) 0.3703(4) 0.5209(2) 0.057 Uiso 1 calc R . N11 N 1.04599(15) 0.2331(3) 0.63903(13) 0.0396(6) Uani 1 d . . C11 C 1.0887(2) 0.3017(3) 0.6019(2) 0.0439(7) Uani 1 d . . H11A H 1.0826(2) 0.2931(3) 0.5579(2) 0.053 Uiso 1 calc R . C12 C 1.1477(2) 0.3949(3) 0.6274(2) 0.0413(7) Uani 1 d . . N13 N 1.1936(2) 0.4543(4) 0.58338(15) 0.0557(8) Uani 1 d . . C14 C 1.2466(2) 0.5409(4) 0.6052(2) 0.0606(10) Uani 1 d . . H14A H 1.2795(2) 0.5823(4) 0.5755(2) 0.073 Uiso 1 calc R . C15 C 1.2557(2) 0.5724(4) 0.6682(2) 0.0563(9) Uani 1 d . . H15A H 1.2926(2) 0.6350(4) 0.6807(2) 0.068 Uiso 1 calc R . C16 C 1.2088(2) 0.5093(4) 0.7130(2) 0.0532(9) Uani 1 d . . H16A H 1.2144(2) 0.5272(4) 0.7563(2) 0.064 Uiso 1 calc R . C17 C 1.1540(2) 0.4198(4) 0.6923(2) 0.0486(8) Uani 1 d . . H17A H 1.1213(2) 0.3763(4) 0.7214(2) 0.058 Uiso 1 calc R . N18 N 0.8943(2) 0.4586(2) 0.64481(13) 0.0387(6) Uani 1 d . . C18 C 0.9380(2) 0.5228(3) 0.6065(2) 0.0428(7) Uani 1 d . . H18A H 0.9376(2) 0.5026(3) 0.5632(2) 0.051 Uiso 1 calc R . C19 C 0.9894(2) 0.6287(3) 0.6293(2) 0.0397(7) Uani 1 d . . N20 N 1.0405(2) 0.6783(4) 0.58603(14) 0.0543(7) Uani 1 d . . C21 C 1.0882(2) 0.7736(4) 0.6064(2) 0.0584(10) Uani 1 d . . H21A H 1.1244(2) 0.8093(4) 0.5772(2) 0.070 Uiso 1 calc R . C22 C 1.0875(2) 0.8219(4) 0.6666(2) 0.0541(8) Uani 1 d . . H22A H 1.1227(2) 0.8877(4) 0.6780(2) 0.065 Uiso 1 calc R . C23 C 1.0342(2) 0.7721(4) 0.7106(2) 0.0493(8) Uani 1 d . . H23A H 1.0318(2) 0.8040(4) 0.7520(2) 0.059 Uiso 1 calc R . C24 C 0.9842(2) 0.6732(4) 0.69142(15) 0.0428(7) Uani 1 d . . H24A H 0.9475(2) 0.6369(4) 0.71996(15) 0.051 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0342(2) 0.0324(2) 0.0399(2) -0.0033(2) -0.0008(2) 0.0003(2) C1 0.0350(14) 0.040(2) 0.045(2) -0.0060(13) 0.0030(13) 0.0060(12) C2 0.046(2) 0.037(2) 0.055(2) 0.003(2) -0.001(2) 0.0019(15) C3 0.052(2) 0.029(2) 0.082(3) -0.005(2) 0.001(2) 0.0016(14) C4 0.055(2) 0.050(2) 0.063(2) -0.025(2) -0.003(2) 0.002(2) C5 0.046(2) 0.056(2) 0.045(2) -0.015(2) 0.0074(14) 0.004(2) C6 0.0343(14) 0.032(2) 0.049(2) -0.0023(13) -0.0010(13) 0.0039(12) C7 0.037(2) 0.039(2) 0.050(2) -0.0033(13) 0.0061(14) 0.0008(13) C8 0.0325(14) 0.043(2) 0.075(2) 0.000(2) 0.002(2) -0.0029(13) C9 0.041(2) 0.048(2) 0.071(2) -0.003(2) -0.018(2) 0.001(2) C10 0.051(2) 0.044(2) 0.046(2) 0.004(2) -0.0107(14) 0.006(2) N11 0.0346(12) 0.043(2) 0.0413(14) 0.0015(12) 0.0022(11) 0.0049(12) C11 0.042(2) 0.051(2) 0.0397(14) -0.001(2) 0.0046(14) 0.0040(14) C12 0.033(2) 0.045(2) 0.046(2) 0.0037(14) 0.0054(12) 0.0056(13) N13 0.048(2) 0.069(2) 0.050(2) 0.0064(15) 0.0058(13) -0.008(2) C14 0.048(2) 0.064(3) 0.069(2) 0.012(2) 0.010(2) -0.010(2) C15 0.046(2) 0.047(2) 0.077(2) -0.002(2) 0.001(2) -0.003(2) C16 0.055(2) 0.050(2) 0.055(2) -0.010(2) 0.004(2) -0.001(2) C17 0.045(2) 0.047(2) 0.053(2) -0.002(2) 0.0104(14) -0.0014(14) N18 0.0389(13) 0.0303(14) 0.0470(14) 0.0019(12) 0.0002(11) 0.0027(11) C18 0.042(2) 0.040(2) 0.046(2) -0.006(2) 0.0011(15) -0.0012(13) C19 0.038(2) 0.036(2) 0.045(2) 0.0036(14) 0.0006(13) -0.0009(13) N20 0.057(2) 0.058(2) 0.047(2) 0.002(2) 0.0072(12) -0.015(2) C21 0.054(2) 0.065(3) 0.056(2) 0.010(2) 0.003(2) -0.018(2) C22 0.052(2) 0.047(2) 0.064(2) 0.004(2) -0.008(2) -0.013(2) C23 0.050(2) 0.051(2) 0.047(2) -0.006(2) -0.0034(15) -0.001(2) C24 0.0423(15) 0.042(2) 0.044(2) 0.004(2) 0.0045(12) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C5 2.035(3) . ? Fe C4 2.038(4) . ? Fe C9 2.040(4) . ? Fe C10 2.041(4) . ? Fe C8 2.044(4) . ? Fe C2 2.045(3) . ? Fe C3 2.052(4) . ? Fe C7 2.054(3) . ? Fe C1 2.056(3) . ? Fe C6 2.058(3) . ? C1 N11 1.408(4) . ? C1 C2 1.420(5) . ? C1 C5 1.426(5) . ? C2 C3 1.420(5) . ? C3 C4 1.404(6) . ? C4 C5 1.426(6) . ? C6 N18 1.395(4) . ? C6 C10 1.427(5) . ? C6 C7 1.440(5) . ? C7 C8 1.414(5) . ? C8 C9 1.418(6) . ? C9 C10 1.418(5) . ? N11 C11 1.269(4) . ? C11 C12 1.475(5) . ? C12 N13 1.342(4) . ? C12 C17 1.387(5) . ? N13 C14 1.337(5) . ? C14 C15 1.368(6) . ? C15 C16 1.380(6) . ? C16 C17 1.370(5) . ? N18 C18 1.268(4) . ? C18 C19 1.474(5) . ? C19 N20 1.339(4) . ? C19 C24 1.383(5) . ? N20 C21 1.338(5) . ? C21 C22 1.359(6) . ? C22 C23 1.372(5) . ? C23 C24 1.381(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe C4 41.0(2) . . ? C5 Fe C9 121.8(2) . . ? C4 Fe C9 105.3(2) . . ? C5 Fe C10 106.2(2) . . ? C4 Fe C10 120.1(2) . . ? C9 Fe C10 40.67(15) . . ? C5 Fe C8 158.31(15) . . ? C4 Fe C8 122.0(2) . . ? C9 Fe C8 40.6(2) . . ? C10 Fe C8 68.56(15) . . ? C5 Fe C2 68.54(15) . . ? C4 Fe C2 67.9(2) . . ? C9 Fe C2 156.8(2) . . ? C10 Fe C2 162.03(14) . . ? C8 Fe C2 122.72(15) . . ? C5 Fe C3 68.5(2) . . ? C4 Fe C3 40.1(2) . . ? C9 Fe C3 120.1(2) . . ? C10 Fe C3 155.3(2) . . ? C8 Fe C3 107.0(2) . . ? C2 Fe C3 40.55(15) . . ? C5 Fe C7 159.28(14) . . ? C4 Fe C7 159.2(2) . . ? C9 Fe C7 68.2(2) . . ? C10 Fe C7 68.76(14) . . ? C8 Fe C7 40.36(14) . . ? C2 Fe C7 109.76(14) . . ? C3 Fe C7 124.6(2) . . ? C5 Fe C1 40.79(14) . . ? C4 Fe C1 68.25(14) . . ? C9 Fe C1 159.6(2) . . ? C10 Fe C1 124.48(14) . . ? C8 Fe C1 159.14(14) . . ? C2 Fe C1 40.51(14) . . ? C3 Fe C1 68.18(14) . . ? C7 Fe C1 124.45(13) . . ? C5 Fe C6 122.19(14) . . ? C4 Fe C6 157.0(2) . . ? C9 Fe C6 68.31(14) . . ? C10 Fe C6 40.75(14) . . ? C8 Fe C6 68.39(13) . . ? C2 Fe C6 126.40(14) . . ? C3 Fe C6 162.3(2) . . ? C7 Fe C6 41.00(13) . . ? C1 Fe C6 109.66(12) . . ? N11 C1 C2 122.4(3) . . ? N11 C1 C5 129.8(3) . . ? C2 C1 C5 107.7(3) . . ? N11 C1 Fe 125.2(2) . . ? C2 C1 Fe 69.3(2) . . ? C5 C1 Fe 68.8(2) . . ? C1 C2 C3 108.4(3) . . ? C1 C2 Fe 70.2(2) . . ? C3 C2 Fe 70.0(2) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Fe 69.4(2) . . ? C2 C3 Fe 69.4(2) . . ? C3 C4 C5 108.8(3) . . ? C3 C4 Fe 70.5(2) . . ? C5 C4 Fe 69.4(2) . . ? C1 C5 C4 107.3(3) . . ? C1 C5 Fe 70.4(2) . . ? C4 C5 Fe 69.6(2) . . ? N18 C6 C10 130.7(3) . . ? N18 C6 C7 121.7(3) . . ? C10 C6 C7 107.5(3) . . ? N18 C6 Fe 127.7(2) . . ? C10 C6 Fe 69.0(2) . . ? C7 C6 Fe 69.4(2) . . ? C8 C7 C6 107.7(3) . . ? C8 C7 Fe 69.4(2) . . ? C6 C7 Fe 69.6(2) . . ? C7 C8 C9 108.4(3) . . ? C7 C8 Fe 70.2(2) . . ? C9 C8 Fe 69.5(2) . . ? C8 C9 C10 108.4(3) . . ? C8 C9 Fe 69.8(2) . . ? C10 C9 Fe 69.7(2) . . ? C9 C10 C6 107.9(3) . . ? C9 C10 Fe 69.6(2) . . ? C6 C10 Fe 70.2(2) . . ? C11 N11 C1 120.3(3) . . ? N11 C11 C12 121.1(3) . . ? N13 C12 C17 122.9(3) . . ? N13 C12 C11 115.3(3) . . ? C17 C12 C11 121.8(3) . . ? C14 N13 C12 116.5(3) . . ? N13 C14 C15 124.2(4) . . ? C14 C15 C16 118.6(4) . . ? C17 C16 C15 118.6(4) . . ? C16 C17 C12 119.1(3) . . ? C18 N18 C6 120.5(3) . . ? N18 C18 C19 121.3(3) . . ? N20 C19 C24 122.9(3) . . ? N20 C19 C18 115.6(3) . . ? C24 C19 C18 121.5(3) . . ? C21 N20 C19 116.2(3) . . ? N20 C21 C22 124.6(4) . . ? C21 C22 C23 119.1(4) . . ? C22 C23 C24 118.0(3) . . ? C23 C24 C19 119.3(3) . . ? _refine_diff_density_max 0.327 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.050 data_Compound_1C _database_code_CSD 196187 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30.50 H24 N4 O0.50 Cl Fe' _chemical_formula_weight 545.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9800(15) _cell_length_b 13.4810(14) _cell_length_c 18.574(2) _cell_angle_alpha 100.235(8) _cell_angle_beta 96.550(10) _cell_angle_gamma 108.479(11) _cell_volume 2522.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 12.50 _exptl_crystal_description blocks _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.04 _diffrn_reflns_number 9231 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8738 _reflns_number_observed 5516 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1012 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7726 _refine_ls_number_parameters 689 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_obs 0.0601 _refine_ls_wR_factor_all 0.1757 _refine_ls_wR_factor_obs 0.1409 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.25678(6) 0.31368(5) 0.51784(4) 0.0396(2) Uani 1 d . . C1 C 0.3044(5) 0.4710(3) 0.5726(3) 0.0435(10) Uani 1 d . . C2 C 0.2812(5) 0.4602(4) 0.4938(3) 0.0508(11) Uani 1 d . . H2A H 0.3402(5) 0.4934(4) 0.4659(3) 0.061 Uiso 1 calc R . C3 C 0.1499(5) 0.3886(4) 0.4661(3) 0.0587(13) Uani 1 d . . H3A H 0.1078(5) 0.3679(4) 0.4166(3) 0.070 Uiso 1 calc R . C4 C 0.0953(5) 0.3549(5) 0.5264(3) 0.0573(13) Uani 1 d . . H4A H 0.0112(5) 0.3076(5) 0.5234(3) 0.069 Uiso 1 calc R . C5 C 0.1899(5) 0.4050(4) 0.5926(3) 0.0511(11) Uani 1 d . . H5A H 0.1791(5) 0.3964(4) 0.6403(3) 0.061 Uiso 1 calc R . C6 C 0.4117(5) 0.2649(4) 0.5451(3) 0.0451(10) Uani 1 d . . C7 C 0.3828(5) 0.2556(4) 0.4669(3) 0.0494(11) Uani 1 d . . H7A H 0.4400(5) 0.2902(4) 0.4386(3) 0.059 Uiso 1 calc R . C8 C 0.2534(5) 0.1856(4) 0.4395(3) 0.0532(12) Uani 1 d . . H8A H 0.2107(5) 0.1661(4) 0.3902(3) 0.064 Uiso 1 calc R . C9 C 0.1994(5) 0.1502(4) 0.5001(3) 0.0563(13) Uani 1 d . . H9A H 0.1153(5) 0.1030(4) 0.4974(3) 0.068 Uiso 1 calc R . C10 C 0.2958(5) 0.1991(4) 0.5655(3) 0.0530(12) Uani 1 d . . H10A H 0.2858(5) 0.1901(4) 0.6132(3) 0.064 Uiso 1 calc R . N11 N 0.4244(4) 0.5392(3) 0.6178(2) 0.0456(9) Uani 1 d . . C11 C 0.4350(5) 0.5560(4) 0.6880(3) 0.0462(10) Uani 1 d . . H11A H 0.3647(5) 0.5198(4) 0.7081(3) 0.055 Uiso 1 calc R . C12 C 0.5541(5) 0.6303(4) 0.7388(3) 0.0486(11) Uani 1 d . . C13 C 0.6672(5) 0.6711(5) 0.7142(3) 0.0593(13) Uani 1 d . . H13A H 0.6701(5) 0.6504(5) 0.6641(3) 0.071 Uiso 1 calc R . C14 C 0.7803(6) 0.7441(5) 0.7629(4) 0.071(2) Uani 1 d . . H14A H 0.8567(6) 0.7720(5) 0.7449(4) 0.085 Uiso 1 calc R . C15 C 0.7773(6) 0.7737(5) 0.8368(4) 0.072(2) Uani 1 d . . H15A H 0.8525(6) 0.8215(5) 0.8688(4) 0.087 Uiso 1 calc R . C16 C 0.6635(6) 0.7336(4) 0.8654(3) 0.0614(14) Uani 1 d . . C17 C 0.6533(8) 0.7618(5) 0.9409(4) 0.076(2) Uani 1 d . . H17A H 0.7261(8) 0.8082(5) 0.9754(4) 0.091 Uiso 1 calc R . C18 C 0.5393(9) 0.7219(6) 0.9630(4) 0.087(2) Uani 1 d . . H18A H 0.5325(9) 0.7400(6) 1.0127(4) 0.104 Uiso 1 calc R . C19 C 0.4312(8) 0.6532(6) 0.9107(4) 0.084(2) Uani 1 d . . H19A H 0.3525(8) 0.6268(6) 0.9269(4) 0.101 Uiso 1 calc R . N20 N 0.4338(5) 0.6229(4) 0.8392(3) 0.0665(13) Uani 1 d . . C21 C 0.5484(5) 0.6605(4) 0.8156(3) 0.0510(12) Uani 1 d . . N22 N 0.5329(4) 0.3287(3) 0.5890(2) 0.0467(9) Uani 1 d . . C22 C 0.5468(5) 0.3459(4) 0.6594(3) 0.0485(11) Uani 1 d . . H22A H 0.4754(5) 0.3161(4) 0.6810(3) 0.058 Uiso 1 calc R . C23 C 0.6724(5) 0.4115(4) 0.7076(3) 0.0451(10) Uani 1 d . . C24 C 0.7839(5) 0.4478(4) 0.6774(3) 0.0531(12) Uani 1 d . . H24A H 0.7796(5) 0.4297(4) 0.6262(3) 0.064 Uiso 1 calc R . C25 C 0.9034(5) 0.5120(5) 0.7241(4) 0.0623(14) Uani 1 d . . H25A H 0.9777(5) 0.5350(5) 0.7033(4) 0.075 Uiso 1 calc R . C26 C 0.9127(6) 0.5411(5) 0.7984(4) 0.067(2) Uani 1 d . . H26A H 0.9927(6) 0.5842(5) 0.8279(4) 0.080 Uiso 1 calc R . C27 C 0.8029(5) 0.5069(4) 0.8314(3) 0.0553(12) Uani 1 d . . C28 C 0.8029(7) 0.5353(5) 0.9090(3) 0.073(2) Uani 1 d . . H28A H 0.8808(7) 0.5773(5) 0.9412(3) 0.087 Uiso 1 calc R . C29 C 0.6924(7) 0.5027(6) 0.9365(4) 0.076(2) Uani 1 d . . H29A H 0.6924(7) 0.5225(6) 0.9871(4) 0.092 Uiso 1 calc R . C30 C 0.5782(7) 0.4383(5) 0.8871(3) 0.070(2) Uani 1 d . . H30A H 0.5023(7) 0.4162(5) 0.9067(3) 0.084 Uiso 1 calc R . N31 N 0.5686(5) 0.4060(4) 0.8144(3) 0.0580(11) Uani 1 d . . C32 C 0.6809(5) 0.4404(4) 0.7862(3) 0.0501(11) Uani 1 d . . Fe' Fe 0.04191(7) 0.24843(6) 0.78782(4) 0.0492(2) Uani 1 d . . C1' C -0.0343(5) 0.0948(4) 0.7212(3) 0.0539(12) Uani 1 d . . C2' C -0.1258(5) 0.1170(5) 0.7643(4) 0.071(2) Uani 1 d . . H2'A H -0.1622(5) 0.0798(5) 0.7988(4) 0.085 Uiso 1 calc R . C3' C -0.1512(6) 0.2075(6) 0.7446(4) 0.079(2) Uani 1 d . . H3'A H -0.2090(6) 0.2381(6) 0.7637(4) 0.095 Uiso 1 calc R . C4' C -0.0754(7) 0.2428(6) 0.6920(4) 0.075(2) Uani 1 d . . H4'A H -0.0741(7) 0.3004(6) 0.6706(4) 0.089 Uiso 1 calc R . C5' C -0.0017(6) 0.1752(5) 0.6774(3) 0.0625(14) Uani 1 d . . H5'A H 0.0577(6) 0.1812(5) 0.6451(3) 0.075 Uiso 1 calc R . C6' C 0.2113(5) 0.2638(4) 0.8562(3) 0.0493(11) Uani 1 d . . C7' C 0.1178(5) 0.2823(5) 0.8990(3) 0.0604(14) Uani 1 d . . H7'A H 0.0841(5) 0.2441(5) 0.9336(3) 0.072 Uiso 1 calc R . C8' C 0.0847(6) 0.3691(5) 0.8798(3) 0.068(2) Uani 1 d . . H8'A H 0.0250(6) 0.3970(5) 0.8993(3) 0.081 Uiso 1 calc R . C9' C 0.1582(6) 0.4059(5) 0.8260(4) 0.0635(14) Uani 1 d . . H9'A H 0.1558(6) 0.4624(5) 0.8041(4) 0.076 Uiso 1 calc R . C10' C 0.2361(5) 0.3411(4) 0.8115(3) 0.0563(12) Uani 1 d . . H10B H 0.2940(5) 0.3479(4) 0.7783(3) 0.068 Uiso 1 calc R . N11' N 0.0137(4) 0.0104(3) 0.7258(2) 0.0526(10) Uani 1 d . . C11' C 0.0726(5) -0.0161(4) 0.6755(3) 0.0497(11) Uani 1 d . . H11B H 0.0834(5) 0.0216(4) 0.6380(3) 0.060 Uiso 1 calc R . C12' C 0.1251(5) -0.1042(4) 0.6736(3) 0.0482(11) Uani 1 d . . C13' C 0.1318(5) -0.1536(4) 0.7316(3) 0.0602(13) Uani 1 d . . H13B H 0.1014(5) -0.1316(4) 0.7742(3) 0.072 Uiso 1 calc R . C14' C 0.1839(7) -0.2371(5) 0.7280(4) 0.073(2) Uani 1 d . . H14B H 0.1881(7) -0.2692(5) 0.7682(4) 0.088 Uiso 1 calc R . C15' C 0.2278(6) -0.2706(5) 0.6664(4) 0.071(2) Uani 1 d . . H15B H 0.2603(6) -0.3268(5) 0.6643(4) 0.085 Uiso 1 calc R . C16' C 0.2254(5) -0.2227(4) 0.6056(3) 0.0577(13) Uani 1 d . . C17' C 0.2745(5) -0.2510(5) 0.5405(4) 0.067(2) Uani 1 d . . H17B H 0.3083(5) -0.3065(5) 0.5358(4) 0.080 Uiso 1 calc R . C18' C 0.2723(6) -0.1984(5) 0.4858(4) 0.069(2) Uani 1 d . . H18B H 0.3058(6) -0.2159(5) 0.4435(4) 0.082 Uiso 1 calc R . C19' C 0.2192(5) -0.1173(5) 0.4938(3) 0.0618(14) Uani 1 d . . H19B H 0.2180(5) -0.0818(5) 0.4553(3) 0.074 Uiso 1 calc R . N20' N 0.1702(4) -0.0868(3) 0.5520(2) 0.0533(10) Uani 1 d . . C21' C 0.1740(4) -0.1378(4) 0.6087(3) 0.0473(11) Uani 1 d . . N22' N 0.2638(4) 0.1816(4) 0.8612(2) 0.0525(10) Uani 1 d . . C22' C 0.3348(5) 0.1624(4) 0.8151(3) 0.0507(11) Uani 1 d . . H22B H 0.3488(5) 0.2018(4) 0.7786(3) 0.061 Uiso 1 calc R . C23' C 0.3956(5) 0.0800(4) 0.8171(3) 0.0512(11) Uani 1 d . . C24' C 0.3980(7) 0.0336(5) 0.8763(3) 0.069(2) Uani 1 d . . H24B H 0.3600(7) 0.0538(5) 0.9160(3) 0.082 Uiso 1 calc R . C25' C 0.4573(8) -0.0448(6) 0.8781(4) 0.087(2) Uani 1 d . . H25B H 0.4594(8) -0.0750(6) 0.9193(4) 0.104 Uiso 1 calc R . C26' C 0.5107(7) -0.0761(6) 0.8207(4) 0.080(2) Uani 1 d . . H26B H 0.5493(7) -0.1281(6) 0.8227(4) 0.096 Uiso 1 calc R . C27' C 0.5097(5) -0.0321(4) 0.7574(4) 0.0624(14) Uani 1 d . . C28' C 0.5602(6) -0.0650(5) 0.6942(4) 0.071(2) Uani 1 d . . H28B H 0.5988(6) -0.1174(5) 0.6933(4) 0.085 Uiso 1 calc R . C29' C 0.5520(6) -0.0199(5) 0.6349(4) 0.071(2) Uani 1 d . . H29B H 0.5839(6) -0.0411(5) 0.5927(4) 0.086 Uiso 1 calc R . C30' C 0.4940(6) 0.0596(5) 0.6387(4) 0.0664(15) Uani 1 d . . H30B H 0.4895(6) 0.0904(5) 0.5979(4) 0.080 Uiso 1 calc R . N31' N 0.4458(4) 0.0931(3) 0.6956(3) 0.0552(10) Uani 1 d . . C32' C 0.4520(5) 0.0480(4) 0.7556(3) 0.0528(12) Uani 1 d . . C40 C 0.2247(41) 0.8592(23) 1.0355(16) 0.234(14) Uani 0.65 d PDU 1 H40A H 0.1806(41) 0.8934(23) 1.0690(16) 0.281 Uiso 0.65 calc PR 1 H40B H 0.3079(41) 0.9117(23) 1.0340(16) 0.281 Uiso 0.65 calc PR 1 Cl1 Cl 0.2481(9) 0.7463(8) 1.0658(5) 0.203(3) Uani 0.65 d PDU 1 Cl2 Cl 0.1281(9) 0.8073(8) 0.9459(5) 0.219(3) Uani 0.65 d PDU 1 C40' C 0.2259(39) 0.8282(20) 1.0483(19) 0.122(10) Uiso 0.35 d PD 2 H40C H 0.3203(39) 0.8579(20) 1.0553(19) 0.146 Uiso 0.35 calc PR 2 H40D H 0.2021(39) 0.8252(20) 1.0968(19) 0.146 Uiso 0.35 calc PR 2 Cl1' Cl 0.1586(23) 0.9125(16) 1.0089(13) 0.260(8) Uani 0.35 d PDU 2 Cl2' Cl 0.1721(19) 0.6995(14) 0.9929(11) 0.234(7) Uani 0.35 d PDU 2 O50 O 0.0400(13) 0.0071(9) 0.8851(6) 0.199(5) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0377(3) 0.0345(3) 0.0418(4) 0.0059(3) 0.0017(3) 0.0095(3) C1 0.048(3) 0.034(2) 0.047(2) 0.007(2) 0.005(2) 0.014(2) C2 0.057(3) 0.041(2) 0.054(3) 0.013(2) 0.002(2) 0.019(2) C3 0.055(3) 0.053(3) 0.060(3) 0.008(2) -0.012(2) 0.018(2) C4 0.037(2) 0.059(3) 0.074(4) 0.007(3) 0.006(2) 0.019(2) C5 0.047(3) 0.051(3) 0.051(3) 0.001(2) 0.008(2) 0.017(2) C6 0.046(2) 0.039(2) 0.049(3) 0.008(2) 0.005(2) 0.017(2) C7 0.051(3) 0.049(3) 0.048(3) 0.004(2) 0.009(2) 0.019(2) C8 0.057(3) 0.043(3) 0.050(3) -0.005(2) -0.004(2) 0.017(2) C9 0.053(3) 0.034(2) 0.068(3) 0.004(2) -0.005(2) 0.007(2) C10 0.060(3) 0.044(3) 0.056(3) 0.013(2) 0.006(2) 0.019(2) N11 0.048(2) 0.039(2) 0.045(2) 0.003(2) 0.000(2) 0.013(2) C11 0.048(3) 0.036(2) 0.053(3) 0.011(2) 0.008(2) 0.013(2) C12 0.058(3) 0.038(2) 0.048(3) 0.009(2) 0.000(2) 0.017(2) C13 0.054(3) 0.059(3) 0.062(3) 0.015(2) -0.001(2) 0.020(3) C14 0.047(3) 0.070(4) 0.085(4) 0.017(3) 0.002(3) 0.011(3) C15 0.067(4) 0.059(3) 0.073(4) 0.006(3) -0.024(3) 0.014(3) C16 0.074(4) 0.044(3) 0.058(3) 0.009(2) -0.013(3) 0.020(3) C17 0.094(5) 0.057(3) 0.057(3) 0.004(3) -0.022(3) 0.017(3) C18 0.123(7) 0.078(4) 0.050(3) 0.010(3) 0.003(4) 0.030(4) C19 0.099(5) 0.082(5) 0.060(4) 0.013(3) 0.019(4) 0.018(4) N20 0.079(3) 0.060(3) 0.050(3) 0.010(2) 0.009(2) 0.012(2) C21 0.060(3) 0.035(2) 0.052(3) 0.008(2) -0.004(2) 0.016(2) N22 0.043(2) 0.047(2) 0.050(2) 0.007(2) 0.003(2) 0.018(2) C22 0.045(3) 0.043(2) 0.055(3) 0.010(2) 0.002(2) 0.015(2) C23 0.044(2) 0.035(2) 0.056(3) 0.010(2) 0.000(2) 0.017(2) C24 0.048(3) 0.052(3) 0.062(3) 0.014(2) 0.004(2) 0.023(2) C25 0.045(3) 0.062(3) 0.080(4) 0.014(3) 0.005(3) 0.022(2) C26 0.051(3) 0.063(3) 0.073(4) 0.004(3) -0.016(3) 0.017(3) C27 0.054(3) 0.047(3) 0.059(3) 0.011(2) -0.005(2) 0.016(2) C28 0.076(4) 0.065(4) 0.060(3) 0.005(3) -0.017(3) 0.017(3) C29 0.089(5) 0.070(4) 0.052(3) 0.011(3) 0.000(3) 0.009(3) C30 0.074(4) 0.073(4) 0.058(3) 0.019(3) 0.015(3) 0.015(3) N31 0.059(3) 0.055(3) 0.053(2) 0.015(2) 0.003(2) 0.011(2) C32 0.053(3) 0.041(2) 0.056(3) 0.012(2) -0.003(2) 0.020(2) Fe' 0.0423(4) 0.0529(4) 0.0481(4) -0.0040(3) 0.0008(3) 0.0216(3) C1' 0.042(2) 0.053(3) 0.056(3) -0.009(2) -0.002(2) 0.017(2) C2' 0.037(3) 0.072(4) 0.084(4) -0.018(3) 0.003(3) 0.014(3) C3' 0.046(3) 0.082(4) 0.094(5) -0.028(4) -0.014(3) 0.036(3) C4' 0.078(4) 0.082(4) 0.061(3) -0.012(3) -0.012(3) 0.049(4) C5' 0.075(4) 0.070(3) 0.044(3) 0.000(2) -0.004(2) 0.041(3) C6' 0.042(2) 0.049(3) 0.047(3) -0.001(2) -0.004(2) 0.014(2) C7' 0.057(3) 0.072(3) 0.044(3) -0.006(2) 0.000(2) 0.024(3) C8' 0.060(3) 0.067(3) 0.064(3) -0.019(3) -0.006(3) 0.030(3) C9' 0.055(3) 0.049(3) 0.084(4) 0.006(3) 0.008(3) 0.022(2) C10' 0.045(3) 0.050(3) 0.071(3) 0.010(2) 0.005(2) 0.016(2) N11' 0.045(2) 0.050(2) 0.055(2) 0.001(2) 0.008(2) 0.012(2) C11' 0.046(3) 0.044(2) 0.052(3) 0.005(2) 0.006(2) 0.011(2) C12' 0.038(2) 0.037(2) 0.059(3) 0.004(2) 0.003(2) 0.006(2) C13' 0.054(3) 0.051(3) 0.067(3) 0.013(2) 0.003(3) 0.008(2) C14' 0.072(4) 0.053(3) 0.091(5) 0.031(3) 0.005(3) 0.013(3) C15' 0.062(3) 0.046(3) 0.106(5) 0.015(3) 0.005(3) 0.025(3) C16' 0.041(2) 0.040(3) 0.082(4) -0.001(2) 0.000(2) 0.013(2) C17' 0.047(3) 0.053(3) 0.094(4) -0.006(3) 0.012(3) 0.019(2) C18' 0.052(3) 0.062(3) 0.077(4) -0.014(3) 0.014(3) 0.015(3) C19' 0.055(3) 0.061(3) 0.058(3) 0.003(3) 0.014(3) 0.010(3) N20' 0.049(2) 0.046(2) 0.058(2) -0.001(2) 0.006(2) 0.014(2) C21' 0.037(2) 0.036(2) 0.060(3) 0.001(2) 0.004(2) 0.007(2) N22' 0.050(2) 0.056(2) 0.050(2) 0.008(2) 0.004(2) 0.020(2) C22' 0.046(3) 0.049(3) 0.055(3) 0.010(2) 0.003(2) 0.017(2) C23' 0.047(3) 0.044(2) 0.058(3) 0.008(2) -0.004(2) 0.015(2) C24' 0.075(4) 0.067(4) 0.061(3) 0.015(3) -0.002(3) 0.026(3) C25' 0.110(6) 0.073(4) 0.083(5) 0.031(4) -0.010(4) 0.041(4) C26' 0.085(4) 0.067(4) 0.095(5) 0.015(4) -0.008(4) 0.045(4) C27' 0.051(3) 0.048(3) 0.083(4) 0.009(3) -0.006(3) 0.019(2) C28' 0.053(3) 0.049(3) 0.105(5) -0.002(3) 0.005(3) 0.023(3) C29' 0.053(3) 0.056(3) 0.096(5) 0.000(3) 0.018(3) 0.014(3) C30' 0.064(3) 0.061(3) 0.076(4) 0.017(3) 0.022(3) 0.021(3) N31' 0.052(2) 0.049(2) 0.068(3) 0.013(2) 0.015(2) 0.021(2) C32' 0.037(2) 0.043(2) 0.072(3) 0.005(2) -0.001(2) 0.013(2) C40 0.234(14) 0.235(14) 0.234(14) 0.053(3) 0.043(3) 0.081(5) Cl1 0.201(3) 0.209(3) 0.201(3) 0.050(2) 0.046(2) 0.071(2) Cl2 0.219(4) 0.223(4) 0.210(4) 0.055(2) 0.037(2) 0.068(2) Cl1' 0.260(8) 0.259(8) 0.260(8) 0.060(3) 0.050(3) 0.088(3) Cl2' 0.231(7) 0.234(7) 0.236(7) 0.049(3) 0.045(2) 0.082(3) O50 0.225(12) 0.153(8) 0.182(10) 0.065(7) 0.026(9) 0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C4 2.033(5) . ? Fe C7 2.035(5) . ? Fe C8 2.038(5) . ? Fe C3 2.040(5) . ? Fe C10 2.042(5) . ? Fe C2 2.043(5) . ? Fe C9 2.044(5) . ? Fe C5 2.044(5) . ? Fe C6 2.052(5) . ? Fe C1 2.053(4) . ? C1 N11 1.411(6) . ? C1 C5 1.422(7) . ? C1 C2 1.429(7) . ? C2 C3 1.431(8) . ? C3 C4 1.409(9) . ? C4 C5 1.419(8) . ? C6 N22 1.398(6) . ? C6 C7 1.424(7) . ? C6 C10 1.436(7) . ? C7 C8 1.408(7) . ? C8 C9 1.417(8) . ? C9 C10 1.418(8) . ? N11 C11 1.268(6) . ? C11 C12 1.468(7) . ? C12 C13 1.356(8) . ? C12 C21 1.426(8) . ? C13 C14 1.408(8) . ? C14 C15 1.365(10) . ? C15 C16 1.401(10) . ? C16 C17 1.413(9) . ? C16 C21 1.430(8) . ? C17 C18 1.340(11) . ? C18 C19 1.389(11) . ? C19 N20 1.326(8) . ? N20 C21 1.354(8) . ? N22 C22 1.269(7) . ? C22 C23 1.467(7) . ? C23 C24 1.389(8) . ? C23 C32 1.427(7) . ? C24 C25 1.406(8) . ? C25 C26 1.349(9) . ? C26 C27 1.399(9) . ? C27 C32 1.421(7) . ? C27 C28 1.423(9) . ? C28 C29 1.347(10) . ? C29 C30 1.390(9) . ? C30 N31 1.324(8) . ? N31 C32 1.371(7) . ? Fe' C8' 2.033(5) . ? Fe' C3' 2.039(5) . ? Fe' C5' 2.041(5) . ? Fe' C9' 2.045(6) . ? Fe' C2' 2.048(6) . ? Fe' C7' 2.049(5) . ? Fe' C4' 2.049(6) . ? Fe' C10' 2.050(5) . ? Fe' C6' 2.058(5) . ? Fe' C1' 2.068(5) . ? C1' N11' 1.409(7) . ? C1' C2' 1.426(8) . ? C1' C5' 1.448(9) . ? C2' C3' 1.431(10) . ? C3' C4' 1.405(11) . ? C4' C5' 1.411(8) . ? C6' N22' 1.414(7) . ? C6' C10' 1.423(8) . ? C6' C7' 1.424(8) . ? C7' C8' 1.420(9) . ? C8' C9' 1.415(10) . ? C9' C10' 1.419(8) . ? N11' C11' 1.259(7) . ? C11' C12' 1.473(7) . ? C12' C13' 1.370(8) . ? C12' C21' 1.433(7) . ? C13' C14' 1.411(9) . ? C14' C15' 1.352(10) . ? C15' C16' 1.398(9) . ? C16' C17' 1.418(9) . ? C16' C21' 1.425(7) . ? C17' C18' 1.341(10) . ? C18' C19' 1.387(9) . ? C19' N20' 1.321(7) . ? N20' C21' 1.360(7) . ? N22' C22' 1.269(7) . ? C22' C23' 1.469(7) . ? C23' C24' 1.360(8) . ? C23' C32' 1.424(8) . ? C24' C25' 1.409(10) . ? C25' C26' 1.342(11) . ? C26' C27' 1.408(10) . ? C27' C28' 1.415(10) . ? C27' C32' 1.417(7) . ? C28' C29' 1.358(10) . ? C29' C30' 1.405(9) . ? C30' N31' 1.309(8) . ? N31' C32' 1.366(7) . ? C40 Cl2 1.76(2) . ? C40 Cl1 1.79(2) . ? C40' Cl2' 1.73(2) . ? C40' Cl1' 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Fe C7 157.5(2) . . ? C4 Fe C8 121.9(2) . . ? C7 Fe C8 40.5(2) . . ? C4 Fe C3 40.5(2) . . ? C7 Fe C3 121.6(2) . . ? C8 Fe C3 106.2(2) . . ? C4 Fe C10 123.5(2) . . ? C7 Fe C10 68.5(2) . . ? C8 Fe C10 68.5(2) . . ? C3 Fe C10 158.8(2) . . ? C4 Fe C2 68.7(2) . . ? C7 Fe C2 106.5(2) . . ? C8 Fe C2 121.6(2) . . ? C3 Fe C2 41.0(2) . . ? C10 Fe C2 159.4(2) . . ? C4 Fe C9 107.5(2) . . ? C7 Fe C9 68.2(2) . . ? C8 Fe C9 40.6(2) . . ? C3 Fe C9 122.1(2) . . ? C10 Fe C9 40.6(2) . . ? C2 Fe C9 158.0(2) . . ? C4 Fe C5 40.7(2) . . ? C7 Fe C5 160.1(2) . . ? C8 Fe C5 158.5(2) . . ? C3 Fe C5 68.5(2) . . ? C10 Fe C5 108.5(2) . . ? C2 Fe C5 68.9(2) . . ? C9 Fe C5 123.2(2) . . ? C4 Fe C6 160.3(2) . . ? C7 Fe C6 40.8(2) . . ? C8 Fe C6 68.6(2) . . ? C3 Fe C6 158.1(2) . . ? C10 Fe C6 41.1(2) . . ? C2 Fe C6 122.2(2) . . ? C9 Fe C6 68.6(2) . . ? C5 Fe C6 124.1(2) . . ? C4 Fe C1 68.2(2) . . ? C7 Fe C1 123.5(2) . . ? C8 Fe C1 158.7(2) . . ? C3 Fe C1 68.4(2) . . ? C10 Fe C1 123.9(2) . . ? C2 Fe C1 40.8(2) . . ? C9 Fe C1 159.7(2) . . ? C5 Fe C1 40.6(2) . . ? C6 Fe C1 108.3(2) . . ? N11 C1 C5 130.0(4) . . ? N11 C1 C2 121.6(4) . . ? C5 C1 C2 108.4(4) . . ? N11 C1 Fe 127.7(3) . . ? C5 C1 Fe 69.4(3) . . ? C2 C1 Fe 69.2(3) . . ? C1 C2 C3 107.0(5) . . ? C1 C2 Fe 69.9(3) . . ? C3 C2 Fe 69.4(3) . . ? C4 C3 C2 108.3(5) . . ? C4 C3 Fe 69.5(3) . . ? C2 C3 Fe 69.6(3) . . ? C3 C4 C5 108.7(5) . . ? C3 C4 Fe 70.0(3) . . ? C5 C4 Fe 70.1(3) . . ? C4 C5 C1 107.6(5) . . ? C4 C5 Fe 69.2(3) . . ? C1 C5 Fe 70.0(3) . . ? N22 C6 C7 123.0(4) . . ? N22 C6 C10 130.2(5) . . ? C7 C6 C10 106.8(4) . . ? N22 C6 Fe 126.5(3) . . ? C7 C6 Fe 69.0(3) . . ? C10 C6 Fe 69.1(3) . . ? C8 C7 C6 108.8(5) . . ? C8 C7 Fe 69.9(3) . . ? C6 C7 Fe 70.2(3) . . ? C7 C8 C9 108.1(4) . . ? C7 C8 Fe 69.7(3) . . ? C9 C8 Fe 69.9(3) . . ? C8 C9 C10 108.1(5) . . ? C8 C9 Fe 69.4(3) . . ? C10 C9 Fe 69.6(3) . . ? C9 C10 C6 108.0(5) . . ? C9 C10 Fe 69.8(3) . . ? C6 C10 Fe 69.8(3) . . ? C11 N11 C1 119.2(4) . . ? N11 C11 C12 122.5(5) . . ? C13 C12 C21 120.0(5) . . ? C13 C12 C11 121.7(5) . . ? C21 C12 C11 118.4(5) . . ? C12 C13 C14 121.4(6) . . ? C15 C14 C13 119.7(6) . . ? C14 C15 C16 121.5(5) . . ? C15 C16 C17 124.3(6) . . ? C15 C16 C21 118.7(5) . . ? C17 C16 C21 116.9(6) . . ? C18 C17 C16 120.3(6) . . ? C17 C18 C19 119.2(7) . . ? N20 C19 C18 123.8(8) . . ? C19 N20 C21 118.2(6) . . ? N20 C21 C12 119.6(5) . . ? N20 C21 C16 121.5(5) . . ? C12 C21 C16 118.8(5) . . ? C22 N22 C6 119.9(4) . . ? N22 C22 C23 121.7(5) . . ? C24 C23 C32 119.2(5) . . ? C24 C23 C22 120.6(5) . . ? C32 C23 C22 120.2(5) . . ? C23 C24 C25 120.1(5) . . ? C26 C25 C24 121.4(6) . . ? C25 C26 C27 120.6(5) . . ? C26 C27 C32 119.6(5) . . ? C26 C27 C28 124.5(5) . . ? C32 C27 C28 115.9(6) . . ? C29 C28 C27 121.2(6) . . ? C28 C29 C30 118.0(6) . . ? N31 C30 C29 125.3(6) . . ? C30 N31 C32 116.7(5) . . ? N31 C32 C27 122.8(5) . . ? N31 C32 C23 118.0(4) . . ? C27 C32 C23 119.1(5) . . ? C8' Fe' C3' 107.3(2) . . ? C8' Fe' C5' 158.0(3) . . ? C3' Fe' C5' 67.7(3) . . ? C8' Fe' C9' 40.6(3) . . ? C3' Fe' C9' 120.9(3) . . ? C5' Fe' C9' 121.9(3) . . ? C8' Fe' C2' 122.4(3) . . ? C3' Fe' C2' 41.0(3) . . ? C5' Fe' C2' 68.9(3) . . ? C9' Fe' C2' 157.4(2) . . ? C8' Fe' C7' 40.7(3) . . ? C3' Fe' C7' 124.7(3) . . ? C5' Fe' C7' 159.5(2) . . ? C9' Fe' C7' 68.3(3) . . ? C2' Fe' C7' 108.8(3) . . ? C8' Fe' C4' 122.0(2) . . ? C3' Fe' C4' 40.2(3) . . ? C5' Fe' C4' 40.3(2) . . ? C9' Fe' C4' 105.6(3) . . ? C2' Fe' C4' 68.9(3) . . ? C7' Fe' C4' 159.4(2) . . ? C8' Fe' C10' 68.1(2) . . ? C3' Fe' C10' 156.4(3) . . ? C5' Fe' C10' 107.3(3) . . ? C9' Fe' C10' 40.5(2) . . ? C2' Fe' C10' 161.1(2) . . ? C7' Fe' C10' 67.9(2) . . ? C4' Fe' C10' 121.0(3) . . ? C8' Fe' C6' 68.5(2) . . ? C3' Fe' C6' 161.5(3) . . ? C5' Fe' C6' 122.9(2) . . ? C9' Fe' C6' 68.5(2) . . ? C2' Fe' C6' 124.8(3) . . ? C7' Fe' C6' 40.6(2) . . ? C4' Fe' C6' 157.4(3) . . ? C10' Fe' C6' 40.5(2) . . ? C8' Fe' C1' 158.9(3) . . ? C3' Fe' C1' 68.0(2) . . ? C5' Fe' C1' 41.3(2) . . ? C9' Fe' C1' 159.7(2) . . ? C2' Fe' C1' 40.5(2) . . ? C7' Fe' C1' 123.8(2) . . ? C4' Fe' C1' 68.6(2) . . ? C10' Fe' C1' 124.5(2) . . ? C6' Fe' C1' 109.0(2) . . ? N11' C1' C2' 123.0(6) . . ? N11' C1' C5' 129.7(5) . . ? C2' C1' C5' 107.3(5) . . ? N11' C1' Fe' 126.1(3) . . ? C2' C1' Fe' 69.0(3) . . ? C5' C1' Fe' 68.4(3) . . ? C1' C2' C3' 107.0(6) . . ? C1' C2' Fe' 70.5(3) . . ? C3' C2' Fe' 69.1(4) . . ? C4' C3' C2' 109.6(5) . . ? C4' C3' Fe' 70.3(3) . . ? C2' C3' Fe' 69.9(3) . . ? C3' C4' C5' 107.7(6) . . ? C3' C4' Fe' 69.5(4) . . ? C5' C4' Fe' 69.5(3) . . ? C4' C5' C1' 108.4(6) . . ? C4' C5' Fe' 70.1(3) . . ? C1' C5' Fe' 70.4(3) . . ? N22' C6' C10' 130.1(5) . . ? N22' C6' C7' 122.8(5) . . ? C10' C6' C7' 107.1(5) . . ? N22' C6' Fe' 126.2(3) . . ? C10' C6' Fe' 69.4(3) . . ? C7' C6' Fe' 69.4(3) . . ? C8' C7' C6' 108.2(6) . . ? C8' C7' Fe' 69.0(3) . . ? C6' C7' Fe' 70.1(3) . . ? C9' C8' C7' 108.4(5) . . ? C9' C8' Fe' 70.2(3) . . ? C7' C8' Fe' 70.3(3) . . ? C8' C9' C10' 107.5(5) . . ? C8' C9' Fe' 69.2(3) . . ? C10' C9' Fe' 69.9(3) . . ? C9' C10' C6' 108.8(5) . . ? C9' C10' Fe' 69.5(3) . . ? C6' C10' Fe' 70.0(3) . . ? C11' N11' C1' 117.7(5) . . ? N11' C11' C12' 122.7(5) . . ? C13' C12' C21' 118.8(5) . . ? C13' C12' C11' 123.0(5) . . ? C21' C12' C11' 118.2(5) . . ? C12' C13' C14' 121.3(6) . . ? C15' C14' C13' 120.2(6) . . ? C14' C15' C16' 121.4(5) . . ? C15' C16' C17' 124.3(5) . . ? C15' C16' C21' 119.0(5) . . ? C17' C16' C21' 116.6(6) . . ? C18' C17' C16' 120.5(5) . . ? C17' C18' C19' 118.6(6) . . ? N20' C19' C18' 124.8(6) . . ? C19' N20' C21' 117.4(5) . . ? N20' C21' C16' 122.1(5) . . ? N20' C21' C12' 118.7(4) . . ? C16' C21' C12' 119.3(5) . . ? C22' N22' C6' 118.7(5) . . ? N22' C22' C23' 122.4(5) . . ? C24' C23' C32' 119.7(5) . . ? C24' C23' C22' 121.1(5) . . ? C32' C23' C22' 119.2(5) . . ? C23' C24' C25' 120.8(7) . . ? C26' C25' C24' 120.3(7) . . ? C25' C26' C27' 121.5(6) . . ? C26' C27' C28' 123.8(6) . . ? C26' C27' C32' 118.5(6) . . ? C28' C27' C32' 117.7(6) . . ? C29' C28' C27' 119.7(5) . . ? C28' C29' C30' 118.4(6) . . ? N31' C30' C29' 124.5(6) . . ? C30' N31' C32' 118.0(5) . . ? N31' C32' C27' 121.7(5) . . ? N31' C32' C23' 119.1(4) . . ? C27' C32' C23' 119.1(5) . . ? Cl2 C40 Cl1 105.8(16) . . ? Cl2' C40' Cl1' 111.9(18) . . ? _refine_diff_density_max 0.719 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.068 data_Compound_7A _database_code_CSD 196188 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H24 N4 Cl4 Fe Pd' _chemical_formula_weight 684.53 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9829(9) _cell_length_b 8.8915(5) _cell_length_c 21.9911(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.042(5) _cell_angle_gamma 90.00 _cell_volume 2614.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 4.78 _cell_measurement_theta_max 12.52 _exptl_crystal_description prisms _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method ? _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.4412 _exptl_absorpt_correction_T_max 0.5112 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.27 _diffrn_reflns_number 4804 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4601 _reflns_number_observed 3494 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 352 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4249 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all 0.1133 _refine_ls_wR_factor_obs 0.0930 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.21034(3) 0.29762(5) 0.43240(2) 0.03394(12) Uani 1 d . . Cl1 Cl 0.09275(11) 0.4182(2) 0.46933(8) 0.0539(4) Uani 1 d . . Cl2 Cl 0.33119(11) 0.1714(2) 0.39979(7) 0.0485(3) Uani 1 d . . Fe Fe 0.38757(5) 0.13754(8) 0.68160(3) 0.0317(2) Uani 1 d . . C1 C 0.2408(4) 0.0746(6) 0.6454(2) 0.0336(10) Uani 1 d . . C2 C 0.2855(4) -0.0045(7) 0.7031(2) 0.0414(11) Uani 1 d . . H2A H 0.2906(4) -0.1084(7) 0.7076(2) 0.050 Uiso 1 calc R . C3 C 0.3207(4) 0.1023(7) 0.7523(2) 0.0437(12) Uani 1 d . . H3A H 0.3535(4) 0.0810(7) 0.7947(2) 0.052 Uiso 1 calc R . C4 C 0.2973(4) 0.2483(7) 0.7254(3) 0.0425(12) Uani 1 d . . H4A H 0.3114(4) 0.3387(7) 0.7475(3) 0.051 Uiso 1 calc R . C5 C 0.2485(3) 0.2326(6) 0.6591(2) 0.0367(10) Uani 1 d . . H5A H 0.2258(3) 0.3103(6) 0.6301(2) 0.044 Uiso 1 calc R . C6 C 0.4704(4) 0.2551(6) 0.6344(2) 0.0388(11) Uani 1 d . . C7 C 0.5205(4) 0.2515(7) 0.7014(3) 0.0460(12) Uani 1 d . . H7A H 0.5380(4) 0.3347(7) 0.7279(3) 0.055 Uiso 1 calc R . C8 C 0.5384(4) 0.1005(8) 0.7199(3) 0.0492(13) Uani 1 d . . H8A H 0.5708(4) 0.0670(8) 0.7608(3) 0.059 Uiso 1 calc R . C9 C 0.4988(4) 0.0071(7) 0.6657(3) 0.0485(13) Uani 1 d . . H9A H 0.5005(4) -0.0974(7) 0.6652(3) 0.058 Uiso 1 calc R . C10 C 0.4566(4) 0.1010(6) 0.6132(2) 0.0386(11) Uani 1 d . . H10A H 0.4252(4) 0.0691(6) 0.5719(2) 0.046 Uiso 1 calc R . N11 N 0.1929(3) 0.0055(5) 0.5866(2) 0.0375(9) Uani 1 d . . C11 C 0.1866(4) 0.0756(6) 0.5357(2) 0.0404(11) Uani 1 d . . H11A H 0.2186(4) 0.1681(6) 0.5379(2) 0.048 Uiso 1 calc R . C12 C 0.1303(4) 0.0158(6) 0.4729(2) 0.0385(11) Uani 1 d . . N13 N 0.1286(3) 0.1025(5) 0.4217(2) 0.0390(9) Uani 1 d . . C14 C 0.0744(4) 0.0576(7) 0.3626(2) 0.0457(13) Uani 1 d . . C15 C 0.0214(4) -0.0758(8) 0.3549(3) 0.055(2) Uani 1 d . . H15A H -0.0176(4) -0.1042(8) 0.3146(3) 0.066 Uiso 1 calc R . C16 C 0.0254(5) -0.1678(8) 0.4064(3) 0.056(2) Uani 1 d . . H16A H -0.0079(5) -0.2596(8) 0.4010(3) 0.067 Uiso 1 calc R . C17 C 0.0804(4) -0.1193(7) 0.4663(3) 0.0485(13) Uani 1 d . . H17A H 0.0837(4) -0.1778(7) 0.5019(3) 0.058 Uiso 1 calc R . C18 C 0.0722(5) 0.1570(9) 0.3080(3) 0.063(2) Uani 1 d . . H18A H 0.0221(5) 0.1220(9) 0.2708(3) 0.094 Uiso 1 d R . H18B H 0.1364(5) 0.1554(9) 0.3004(3) 0.094 Uiso 1 d R . H18C H 0.0567(5) 0.2579(9) 0.3175(3) 0.094 Uiso 1 d R . N19 N 0.4421(3) 0.3890(5) 0.6004(2) 0.0417(10) Uani 1 d . . C19 C 0.3961(4) 0.3796(6) 0.5416(3) 0.0416(11) Uani 1 d . . H19A H 0.3814(4) 0.2848(6) 0.5234(3) 0.050 Uiso 1 calc R . C20 C 0.3647(4) 0.5136(6) 0.5009(3) 0.0403(11) Uani 1 d . . N21 N 0.2913(3) 0.4941(5) 0.4463(2) 0.0372(9) Uani 1 d . . C22 C 0.2626(5) 0.6084(7) 0.4043(3) 0.0500(14) Uani 1 d . . C23 C 0.3089(6) 0.7481(7) 0.4183(4) 0.060(2) Uani 1 d . . H23A H 0.2905(6) 0.8263(7) 0.3891(4) 0.072 Uiso 1 calc R . C24 C 0.3814(6) 0.7708(7) 0.4748(4) 0.062(2) Uani 1 d . . H24A H 0.4099(6) 0.8654(7) 0.4850(4) 0.075 Uiso 1 calc R . C25 C 0.4119(5) 0.6520(7) 0.5166(3) 0.0529(14) Uani 1 d . . H25A H 0.4628(5) 0.6644(7) 0.5544(3) 0.063 Uiso 1 calc R . C26 C 0.1809(5) 0.5808(9) 0.3440(3) 0.062(2) Uani 1 d . . H26A H 0.1698(5) 0.6704(9) 0.3184(3) 0.093 Uiso 1 d R . H26B H 0.1206(5) 0.5543(9) 0.3538(3) 0.093 Uiso 1 d R . H26C H 0.2000(5) 0.5002(9) 0.3209(3) 0.093 Uiso 1 d R . C30 C 0.1483(5) 0.6563(8) 0.6285(3) 0.058(2) Uani 1 d . . H30A H 0.1300(5) 0.7618(8) 0.6228(3) 0.070 Uiso 1 calc R . H30B H 0.0993(5) 0.5991(8) 0.5965(3) 0.070 Uiso 1 calc R . Cl3 Cl 0.26701(14) 0.6307(2) 0.61844(9) 0.0651(4) Uani 1 d . . Cl4 Cl 0.1474(2) 0.5978(3) 0.70403(14) 0.1103(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0359(2) 0.0363(2) 0.0314(2) -0.0002(2) 0.01251(13) 0.0045(2) Cl1 0.0418(7) 0.0609(9) 0.0642(8) -0.0175(7) 0.0237(6) 0.0015(6) Cl2 0.0512(7) 0.0473(8) 0.0550(7) -0.0011(6) 0.0282(6) 0.0101(6) Fe 0.0310(3) 0.0337(4) 0.0295(3) -0.0027(3) 0.0075(3) -0.0002(3) C1 0.032(2) 0.040(3) 0.030(2) 0.001(2) 0.011(2) -0.001(2) C2 0.045(3) 0.041(3) 0.037(3) 0.006(2) 0.011(2) -0.005(2) C3 0.049(3) 0.057(3) 0.026(2) -0.004(2) 0.013(2) -0.007(3) C4 0.040(3) 0.046(3) 0.044(3) -0.013(2) 0.017(2) -0.001(2) C5 0.030(2) 0.035(3) 0.044(3) -0.003(2) 0.010(2) 0.000(2) C6 0.032(2) 0.042(3) 0.044(3) -0.006(2) 0.014(2) -0.006(2) C7 0.032(2) 0.057(3) 0.046(3) -0.006(2) 0.005(2) -0.003(2) C8 0.034(3) 0.061(4) 0.046(3) 0.005(3) 0.002(2) 0.007(2) C9 0.042(3) 0.049(3) 0.057(3) 0.000(3) 0.018(2) 0.014(3) C10 0.034(2) 0.047(3) 0.038(2) -0.010(2) 0.015(2) 0.001(2) N11 0.037(2) 0.035(2) 0.037(2) -0.001(2) 0.005(2) -0.003(2) C11 0.045(3) 0.041(3) 0.033(2) -0.002(2) 0.008(2) -0.011(2) C12 0.032(2) 0.045(3) 0.039(3) -0.006(2) 0.010(2) 0.000(2) N13 0.038(2) 0.044(2) 0.034(2) -0.009(2) 0.009(2) 0.004(2) C14 0.038(3) 0.062(4) 0.032(2) -0.014(2) 0.002(2) 0.008(3) C15 0.038(3) 0.069(4) 0.048(3) -0.026(3) -0.002(2) 0.003(3) C16 0.050(3) 0.057(4) 0.059(3) -0.017(3) 0.013(3) -0.012(3) C17 0.044(3) 0.051(3) 0.048(3) -0.009(3) 0.010(2) -0.008(3) C18 0.062(4) 0.087(5) 0.032(3) -0.007(3) 0.001(2) 0.014(4) N19 0.040(2) 0.041(3) 0.046(2) -0.006(2) 0.016(2) -0.004(2) C19 0.040(3) 0.035(3) 0.051(3) 0.004(2) 0.015(2) -0.001(2) C20 0.040(3) 0.039(3) 0.050(3) 0.001(2) 0.027(2) -0.001(2) N21 0.045(2) 0.029(2) 0.045(2) 0.005(2) 0.024(2) 0.007(2) C22 0.057(3) 0.048(3) 0.056(3) 0.012(3) 0.033(3) 0.018(3) C23 0.075(4) 0.043(3) 0.078(4) 0.018(3) 0.047(4) 0.015(3) C24 0.072(4) 0.038(3) 0.093(5) -0.003(3) 0.051(4) -0.005(3) C25 0.057(3) 0.049(3) 0.063(4) -0.008(3) 0.033(3) -0.008(3) C26 0.067(4) 0.070(4) 0.050(3) 0.018(3) 0.019(3) 0.020(4) C30 0.047(3) 0.055(4) 0.070(4) 0.008(3) 0.012(3) 0.000(3) Cl3 0.0663(10) 0.0617(10) 0.0738(10) -0.0111(8) 0.0305(8) 0.0015(8) Cl4 0.138(2) 0.105(2) 0.121(2) 0.048(2) 0.091(2) 0.050(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N13 2.053(5) . ? Pd N21 2.055(5) . ? Pd Cl1 2.3012(14) . ? Pd Cl2 2.3110(13) . ? Fe C10 2.037(5) . ? Fe C5 2.044(5) . ? Fe C7 2.048(6) . ? Fe C1 2.050(5) . ? Fe C9 2.050(5) . ? Fe C4 2.051(5) . ? Fe C6 2.053(5) . ? Fe C8 2.055(5) . ? Fe C3 2.059(5) . ? Fe C2 2.062(5) . ? C1 N11 1.411(6) . ? C1 C2 1.424(7) . ? C1 C5 1.434(7) . ? C2 C3 1.415(8) . ? C3 C4 1.424(9) . ? C4 C5 1.423(7) . ? C6 N19 1.400(7) . ? C6 C7 1.434(7) . ? C6 C10 1.442(8) . ? C7 C8 1.403(9) . ? C8 C9 1.423(9) . ? C9 C10 1.407(8) . ? N11 C11 1.262(7) . ? C11 C12 1.475(7) . ? C12 N13 1.358(7) . ? C12 C17 1.375(8) . ? N13 C14 1.358(6) . ? C14 C15 1.383(10) . ? C14 C18 1.483(9) . ? C15 C16 1.385(10) . ? C16 C17 1.384(8) . ? N19 C19 1.266(7) . ? C19 C20 1.478(8) . ? C20 N21 1.342(7) . ? C20 C25 1.391(8) . ? N21 C22 1.354(7) . ? C22 C23 1.393(10) . ? C22 C26 1.495(10) . ? C23 C24 1.369(11) . ? C24 C25 1.383(10) . ? C30 Cl4 1.745(7) . ? C30 Cl3 1.753(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Pd N21 177.9(2) . . ? N13 Pd Cl1 90.16(12) . . ? N21 Pd Cl1 88.32(12) . . ? N13 Pd Cl2 89.26(12) . . ? N21 Pd Cl2 92.19(12) . . ? Cl1 Pd Cl2 177.39(6) . . ? C10 Fe C5 120.7(2) . . ? C10 Fe C7 68.8(2) . . ? C5 Fe C7 125.9(2) . . ? C10 Fe C1 107.9(2) . . ? C5 Fe C1 41.0(2) . . ? C7 Fe C1 163.8(2) . . ? C10 Fe C9 40.3(2) . . ? C5 Fe C9 155.3(2) . . ? C7 Fe C9 68.2(3) . . ? C1 Fe C9 120.2(2) . . ? C10 Fe C4 156.0(2) . . ? C5 Fe C4 40.7(2) . . ? C7 Fe C4 108.0(2) . . ? C1 Fe C4 68.2(2) . . ? C9 Fe C4 162.5(2) . . ? C10 Fe C6 41.3(2) . . ? C5 Fe C6 107.7(2) . . ? C7 Fe C6 40.9(2) . . ? C1 Fe C6 126.3(2) . . ? C9 Fe C6 68.5(2) . . ? C4 Fe C6 120.6(2) . . ? C10 Fe C8 68.0(2) . . ? C5 Fe C8 162.7(2) . . ? C7 Fe C8 40.0(3) . . ? C1 Fe C8 154.9(2) . . ? C9 Fe C8 40.6(2) . . ? C4 Fe C8 125.7(2) . . ? C6 Fe C8 68.0(2) . . ? C10 Fe C3 162.0(2) . . ? C5 Fe C3 68.6(2) . . ? C7 Fe C3 120.0(2) . . ? C1 Fe C3 68.1(2) . . ? C9 Fe C3 125.3(3) . . ? C4 Fe C3 40.5(2) . . ? C6 Fe C3 155.1(2) . . ? C8 Fe C3 107.8(2) . . ? C10 Fe C2 125.5(2) . . ? C5 Fe C2 68.6(2) . . ? C7 Fe C2 154.2(2) . . ? C1 Fe C2 40.5(2) . . ? C9 Fe C2 107.7(3) . . ? C4 Fe C2 67.9(2) . . ? C6 Fe C2 163.5(2) . . ? C8 Fe C2 120.3(2) . . ? C3 Fe C2 40.2(2) . . ? N11 C1 C2 124.6(5) . . ? N11 C1 C5 127.2(5) . . ? C2 C1 C5 108.1(4) . . ? N11 C1 Fe 128.8(3) . . ? C2 C1 Fe 70.2(3) . . ? C5 C1 Fe 69.3(3) . . ? C3 C2 C1 108.2(5) . . ? C3 C2 Fe 69.8(3) . . ? C1 C2 Fe 69.3(3) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 Fe 70.0(3) . . ? C4 C3 Fe 69.4(3) . . ? C5 C4 C3 108.6(5) . . ? C5 C4 Fe 69.4(3) . . ? C3 C4 Fe 70.0(3) . . ? C4 C5 C1 107.1(5) . . ? C4 C5 Fe 69.9(3) . . ? C1 C5 Fe 69.7(3) . . ? N19 C6 C7 123.0(5) . . ? N19 C6 C10 130.2(5) . . ? C7 C6 C10 106.8(5) . . ? N19 C6 Fe 126.2(4) . . ? C7 C6 Fe 69.3(3) . . ? C10 C6 Fe 68.7(3) . . ? C8 C7 C6 108.1(5) . . ? C8 C7 Fe 70.3(3) . . ? C6 C7 Fe 69.7(3) . . ? C7 C8 C9 108.8(5) . . ? C7 C8 Fe 69.7(3) . . ? C9 C8 Fe 69.5(3) . . ? C10 C9 C8 107.9(5) . . ? C10 C9 Fe 69.4(3) . . ? C8 C9 Fe 69.9(3) . . ? C9 C10 C6 108.4(5) . . ? C9 C10 Fe 70.4(3) . . ? C6 C10 Fe 70.0(3) . . ? C11 N11 C1 119.2(5) . . ? N11 C11 C12 122.2(5) . . ? N13 C12 C17 121.5(5) . . ? N13 C12 C11 116.6(5) . . ? C17 C12 C11 121.9(5) . . ? C12 N13 C14 119.7(5) . . ? C12 N13 Pd 120.7(3) . . ? C14 N13 Pd 119.6(4) . . ? N13 C14 C15 119.8(6) . . ? N13 C14 C18 118.2(6) . . ? C15 C14 C18 121.9(5) . . ? C14 C15 C16 121.0(5) . . ? C17 C16 C15 118.2(6) . . ? C12 C17 C16 119.7(6) . . ? C19 N19 C6 117.9(5) . . ? N19 C19 C20 122.5(5) . . ? N21 C20 C25 121.3(5) . . ? N21 C20 C19 116.8(5) . . ? C25 C20 C19 121.9(5) . . ? C20 N21 C22 120.6(5) . . ? C20 N21 Pd 119.1(3) . . ? C22 N21 Pd 119.8(4) . . ? N21 C22 C23 119.5(6) . . ? N21 C22 C26 118.7(6) . . ? C23 C22 C26 121.8(6) . . ? C24 C23 C22 120.3(6) . . ? C23 C24 C25 119.5(6) . . ? C24 C25 C20 118.6(6) . . ? Cl4 C30 Cl3 110.6(4) . . ? _refine_diff_density_max 0.507 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.092 data_Compound_6B _database_code_CSD 196189 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17.50 H18 Cl2 Fe N2 Pd' _chemical_formula_weight 489.49 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0625(13) _cell_length_b 22.804(3) _cell_length_c 15.739(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.264(12) _cell_angle_gamma 90.00 _cell_volume 3582.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 12.70 _exptl_crystal_description 'platy prisms' _exptl_crystal_colour 'Very dark orange' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method ? _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 2.112 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2320 _exptl_absorpt_correction_T_max 0.6940 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.83 _diffrn_reflns_number 6633 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6256 _reflns_number_observed 4437 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 534 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5722 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_obs 0.0436 _refine_ls_wR_factor_all 0.1002 _refine_ls_wR_factor_obs 0.0854 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 1.039 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.52266(5) 0.25538(2) 0.78277(3) 0.03456(11) Uani 1 d . . Fe Fe 0.50790(11) 0.43366(3) 0.65597(5) 0.0411(2) Uani 1 d . . Cl Cl 0.7299(2) 0.28815(7) 0.75561(12) 0.0499(4) Uani 1 d . . C1 C 0.6205(7) 0.1930(3) 0.8580(5) 0.048(2) Uani 1 d . . H1A H 0.7165(11) 0.1949(17) 0.8530(29) 0.073 Uiso 1 calc R . H1B H 0.5860(42) 0.1542(3) 0.8396(25) 0.073 Uiso 1 calc R . H1C H 0.6063(48) 0.1996(15) 0.9177(7) 0.073 Uiso 1 calc R . C2 C 0.4101(7) 0.3562(2) 0.6364(4) 0.0392(14) Uani 1 d . . C3 C 0.3246(9) 0.4032(3) 0.6049(4) 0.050(2) Uani 1 d . . H3A H 0.2411(9) 0.4133(3) 0.6231(4) 0.060 Uiso 1 calc R . C4 C 0.3892(10) 0.4323(3) 0.5404(4) 0.059(2) Uani 1 d . . H4A H 0.3551(10) 0.4654(3) 0.5081(4) 0.071 Uiso 1 calc R . C5 C 0.5122(9) 0.4036(3) 0.5328(4) 0.054(2) Uani 1 d . . H5A H 0.5737(9) 0.4139(3) 0.4942(4) 0.064 Uiso 1 calc R . C6 C 0.5279(8) 0.3564(3) 0.5932(4) 0.045(2) Uani 1 d . . H6A H 0.6017(8) 0.3303(3) 0.6029(4) 0.053 Uiso 1 calc R . C7 C 0.5729(8) 0.4386(3) 0.7838(4) 0.0448(15) Uani 1 d . . H7A H 0.5702(8) 0.4080(3) 0.8246(4) 0.054 Uiso 1 calc R . C8 C 0.6806(8) 0.4498(3) 0.7367(4) 0.050(2) Uani 1 d . . H8A H 0.7615(8) 0.4280(3) 0.7396(4) 0.060 Uiso 1 calc R . C9 C 0.6465(11) 0.4989(3) 0.6850(5) 0.066(3) Uani 1 d . . H9A H 0.7014(11) 0.5161(3) 0.6470(5) 0.080 Uiso 1 calc R . C10 C 0.5198(12) 0.5183(3) 0.6982(6) 0.074(3) Uani 1 d . . H10B H 0.4740(12) 0.5511(3) 0.6710(6) 0.089 Uiso 1 calc R . C11 C 0.4694(9) 0.4800(3) 0.7610(5) 0.056(2) Uani 1 d . . H11B H 0.3852(9) 0.4822(3) 0.7821(5) 0.067 Uiso 1 calc R . N12 N 0.3880(6) 0.3147(2) 0.7014(3) 0.0372(11) Uani 1 d . . C12 C 0.2656(7) 0.3079(2) 0.7155(4) 0.0422(14) Uani 1 d . . H12B H 0.1963(7) 0.3309(2) 0.6853(4) 0.051 Uiso 1 calc R . C13 C 0.2349(7) 0.2647(2) 0.7779(4) 0.0399(13) Uani 1 d . . N14 N 0.3391(6) 0.2311(2) 0.8152(3) 0.0379(11) Uani 1 d . . C15 C 0.3103(8) 0.1897(3) 0.8721(4) 0.0456(15) Uani 1 d . . H15B H 0.3816(8) 0.1667(3) 0.9001(4) 0.055 Uiso 1 calc R . C16 C 0.1822(9) 0.1795(3) 0.8911(5) 0.058(2) Uani 1 d . . H16B H 0.1664(9) 0.1493(3) 0.9301(5) 0.069 Uiso 1 calc R . C17 C 0.0779(8) 0.2128(3) 0.8540(5) 0.054(2) Uani 1 d . . H17B H -0.0106(8) 0.2060(3) 0.8667(5) 0.064 Uiso 1 calc R . C18 C 0.1036(7) 0.2571(3) 0.7971(5) 0.051(2) Uani 1 d . . H18B H 0.0332(7) 0.2817(3) 0.7718(5) 0.061 Uiso 1 calc R . Pd' Pd 0.88112(5) 0.49245(2) 0.15231(3) 0.03995(13) Uani 1 d . . Fe' Fe 0.68158(9) 0.62593(3) -0.04648(5) 0.0342(2) Uani 1 d . . Cl' Cl 0.9257(3) 0.58269(8) 0.21598(12) 0.0728(6) Uani 1 d . . C1' C 0.9165(12) 0.4570(4) 0.2705(4) 0.075(3) Uani 1 d . . H1'1 H 0.9417(82) 0.4881(6) 0.3125(8) 0.112 Uiso 1 calc R . H1'2 H 0.9896(56) 0.4285(27) 0.2720(15) 0.112 Uiso 1 calc R . H1'3 H 0.8354(27) 0.4373(31) 0.2843(21) 0.112 Uiso 1 calc R . C2' C 0.8400(6) 0.5702(3) -0.0291(4) 0.0359(12) Uani 1 d . . C3' C 0.7996(7) 0.5802(3) -0.1193(4) 0.0404(13) Uani 1 d . . H3'A H 0.7711(7) 0.5512(3) -0.1610(4) 0.048 Uiso 1 calc R . C4' C 0.8105(7) 0.6412(3) -0.1341(5) 0.049(2) Uani 1 d . . H4'A H 0.7897(7) 0.6603(3) -0.1877(5) 0.058 Uiso 1 calc R . C5' C 0.8580(8) 0.6688(3) -0.0550(5) 0.052(2) Uani 1 d . . H5'A H 0.8752(8) 0.7095(3) -0.0471(5) 0.063 Uiso 1 calc R . C6' C 0.8751(7) 0.6258(3) 0.0094(5) 0.0442(14) Uani 1 d . . H6'A H 0.9048(7) 0.6325(3) 0.0683(5) 0.053 Uiso 1 calc R . C7' C 0.5314(7) 0.5888(3) 0.0115(4) 0.0430(14) Uani 1 d . . H7'A H 0.5362(7) 0.5524(3) 0.0413(4) 0.052 Uiso 1 calc R . C8' C 0.5667(7) 0.6439(3) 0.0479(5) 0.050(2) Uani 1 d . . H8'A H 0.5990(7) 0.6510(3) 0.1064(5) 0.060 Uiso 1 calc R . C9' C 0.5463(9) 0.6869(3) -0.0164(6) 0.062(2) Uani 1 d . . H9'A H 0.5615(9) 0.7278(3) -0.0091(6) 0.074 Uiso 1 calc R . C10' C 0.4990(8) 0.6583(4) -0.0943(5) 0.058(2) Uani 1 d . . H10A H 0.4785(8) 0.6767(4) -0.1485(5) 0.070 Uiso 1 calc R . C11' C 0.4874(7) 0.5967(3) -0.0774(4) 0.0469(15) Uani 1 d . . H11A H 0.4564(7) 0.5671(3) -0.1176(4) 0.056 Uiso 1 calc R . N12' N 0.8430(5) 0.5165(2) 0.0151(3) 0.0338(10) Uani 1 d . . C12' C 0.8295(6) 0.4698(3) -0.0305(4) 0.0392(13) Uani 1 d . . H12A H 0.8230(6) 0.4725(3) -0.0911(4) 0.047 Uiso 1 calc R . C13' C 0.8243(6) 0.4125(2) 0.0103(4) 0.0376(12) Uani 1 d . . N14' N 0.8442(6) 0.4114(2) 0.0970(4) 0.0411(12) Uani 1 d . . C15' C 0.8419(7) 0.3598(3) 0.1362(5) 0.050(2) Uani 1 d . . H15A H 0.8589(7) 0.3582(3) 0.1969(5) 0.060 Uiso 1 calc R . C16' C 0.8147(9) 0.3076(3) 0.0895(6) 0.063(2) Uani 1 d . . H16A H 0.8082(9) 0.2715(3) 0.1189(6) 0.076 Uiso 1 calc R . C17' C 0.7977(7) 0.3089(3) 0.0026(6) 0.054(2) Uani 1 d . . H17A H 0.7852(7) 0.2735(3) -0.0294(6) 0.065 Uiso 1 calc R . C18' C 0.7991(7) 0.3625(3) -0.0387(5) 0.050(2) Uani 1 d . . H18A H 0.7830(7) 0.3648(3) -0.0994(5) 0.060 Uiso 1 calc R . C20 C 0.1094(11) 0.6029(4) 0.4189(6) 0.072(2) Uani 1 d . . H20A H 0.1984(11) 0.6077(4) 0.3992(6) 0.087 Uiso 1 calc R . H20B H 0.0500(11) 0.5825(4) 0.3734(6) 0.087 Uiso 1 calc R . Cl2 Cl 0.0431(3) 0.67120(10) 0.4384(2) 0.0811(6) Uani 1 d . . Cl3 Cl 0.1247(5) 0.5612(2) 0.5137(3) 0.1347(15) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0355(2) 0.0300(2) 0.0381(2) -0.0028(2) 0.0042(2) 0.0004(2) Fe 0.0579(6) 0.0331(4) 0.0305(4) -0.0002(3) -0.0012(4) -0.0069(4) Cl 0.0394(9) 0.0541(8) 0.0585(9) -0.0034(7) 0.0152(7) -0.0011(7) C1 0.036(4) 0.047(3) 0.059(4) 0.005(3) -0.008(3) 0.004(3) C2 0.048(4) 0.035(3) 0.033(3) -0.002(2) -0.001(3) -0.006(3) C3 0.061(5) 0.043(3) 0.041(3) 0.006(3) -0.010(3) -0.007(3) C4 0.090(6) 0.040(3) 0.042(3) 0.008(3) -0.011(4) -0.017(4) C5 0.085(6) 0.045(3) 0.030(3) -0.009(2) 0.004(3) -0.018(4) C6 0.062(5) 0.040(3) 0.031(3) -0.008(2) 0.004(3) -0.010(3) C7 0.060(4) 0.047(3) 0.027(3) -0.006(2) 0.004(3) -0.006(3) C8 0.056(5) 0.061(4) 0.033(3) -0.014(3) 0.002(3) -0.014(3) C9 0.104(7) 0.052(4) 0.042(3) -0.001(3) 0.004(4) -0.040(5) C10 0.115(9) 0.035(3) 0.063(5) -0.010(3) -0.027(5) 0.008(4) C11 0.064(5) 0.052(4) 0.050(4) -0.021(3) -0.001(3) 0.005(3) N12 0.043(3) 0.031(2) 0.036(2) -0.002(2) -0.001(2) -0.002(2) C12 0.039(4) 0.033(3) 0.052(3) 0.000(2) 0.000(3) -0.002(2) C13 0.036(3) 0.036(3) 0.047(3) -0.003(2) 0.003(3) 0.000(2) N14 0.044(3) 0.034(2) 0.036(2) 0.000(2) 0.002(2) -0.002(2) C15 0.047(4) 0.043(3) 0.046(3) 0.011(3) 0.003(3) -0.007(3) C16 0.059(5) 0.056(4) 0.059(4) 0.014(3) 0.011(4) -0.015(3) C17 0.045(4) 0.063(4) 0.056(4) 0.002(3) 0.017(3) -0.008(3) C18 0.043(4) 0.048(3) 0.060(4) -0.002(3) 0.005(3) 0.001(3) Pd' 0.0378(3) 0.0456(2) 0.0366(2) 0.0002(2) 0.0056(2) 0.0083(2) Fe' 0.0304(5) 0.0342(3) 0.0381(4) 0.0013(3) 0.0046(4) 0.0002(3) Cl' 0.112(2) 0.0546(9) 0.0487(9) -0.0148(7) -0.0013(11) 0.0107(10) C1' 0.118(9) 0.076(5) 0.031(3) 0.008(3) 0.007(4) 0.011(5) C2' 0.023(3) 0.045(3) 0.040(3) 0.005(2) 0.005(2) 0.002(2) C3' 0.034(3) 0.048(3) 0.041(3) 0.003(2) 0.014(3) -0.001(3) C4' 0.042(4) 0.051(3) 0.055(4) 0.022(3) 0.014(3) 0.006(3) C5' 0.038(4) 0.046(3) 0.076(5) 0.009(3) 0.017(4) -0.003(3) C6' 0.029(3) 0.043(3) 0.059(4) 0.000(3) 0.000(3) -0.009(3) C7' 0.031(4) 0.045(3) 0.055(4) -0.002(3) 0.014(3) -0.002(3) C8' 0.038(4) 0.056(4) 0.060(4) -0.021(3) 0.016(3) -0.001(3) C9' 0.050(4) 0.047(3) 0.089(6) -0.007(4) 0.013(4) 0.012(3) C10' 0.041(4) 0.074(4) 0.059(4) 0.016(4) 0.006(3) 0.016(4) C11' 0.022(3) 0.068(4) 0.049(4) -0.014(3) -0.001(3) -0.007(3) N12' 0.019(2) 0.039(2) 0.043(2) -0.001(2) 0.003(2) 0.002(2) C12' 0.027(3) 0.046(3) 0.043(3) 0.002(2) -0.002(3) 0.001(2) C13' 0.026(3) 0.039(3) 0.047(3) -0.002(2) 0.003(3) 0.004(2) N14' 0.032(3) 0.037(2) 0.055(3) 0.003(2) 0.007(2) 0.003(2) C15' 0.039(4) 0.059(4) 0.056(4) 0.011(3) 0.017(3) 0.003(3) C16' 0.054(5) 0.045(3) 0.092(6) 0.014(4) 0.019(4) -0.002(3) C17' 0.033(4) 0.039(3) 0.088(6) -0.004(3) 0.001(4) -0.002(3) C18' 0.035(4) 0.049(3) 0.062(4) -0.001(3) -0.008(3) 0.003(3) C20 0.065(6) 0.092(6) 0.059(5) -0.004(4) 0.004(4) 0.012(5) Cl2 0.079(2) 0.0736(12) 0.089(2) -0.0111(11) 0.0056(13) -0.0016(11) Cl3 0.139(4) 0.126(3) 0.140(3) 0.063(2) 0.021(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.025(6) . ? Pd N14 2.053(6) . ? Pd N12 2.206(5) . ? Pd Cl 2.306(2) . ? Fe C2 2.026(6) . ? Fe C3 2.038(8) . ? Fe C7 2.039(6) . ? Fe C11 2.040(7) . ? Fe C10 2.041(7) . ? Fe C6 2.042(6) . ? Fe C4 2.046(7) . ? Fe C9 2.051(7) . ? Fe C8 2.053(7) . ? Fe C5 2.062(6) . ? C2 C3 1.422(10) . ? C2 N12 1.433(8) . ? C2 C6 1.439(10) . ? C3 C4 1.436(11) . ? C4 C5 1.419(13) . ? C5 C6 1.432(9) . ? C7 C8 1.411(11) . ? C7 C11 1.418(11) . ? C8 C9 1.401(11) . ? C9 C10 1.390(15) . ? C10 C11 1.458(13) . ? N12 C12 1.287(9) . ? C12 C13 1.451(9) . ? C13 N14 1.369(8) . ? C13 C18 1.404(10) . ? N14 C15 1.358(8) . ? C15 C16 1.380(11) . ? C16 C17 1.365(12) . ? C17 C18 1.394(10) . ? Pd' C1' 2.018(7) . ? Pd' N14' 2.057(5) . ? Pd' N12' 2.214(5) . ? Pd' Cl' 2.308(2) . ? Fe' C2' 2.030(6) . ? Fe' C6' 2.032(7) . ? Fe' C10' 2.034(8) . ? Fe' C8' 2.037(7) . ? Fe' C3' 2.040(6) . ? Fe' C4' 2.040(7) . ? Fe' C9' 2.042(7) . ? Fe' C5' 2.045(7) . ? Fe' C7' 2.045(7) . ? Fe' C11' 2.064(7) . ? C2' N12' 1.407(8) . ? C2' C6' 1.430(9) . ? C2' C3' 1.445(9) . ? C3' C4' 1.417(9) . ? C4' C5' 1.423(11) . ? C5' C6' 1.404(10) . ? C7' C8' 1.409(9) . ? C7' C11' 1.426(10) . ? C8' C9' 1.405(12) . ? C9' C10' 1.416(12) . ? C10' C11' 1.437(11) . ? N12' C12' 1.282(8) . ? C12' C13' 1.461(8) . ? C13' N14' 1.354(9) . ? C13' C18' 1.381(9) . ? N14' C15' 1.329(9) . ? C15' C16' 1.407(11) . ? C16' C17' 1.358(13) . ? C17' C18' 1.385(10) . ? C20 Cl2 1.737(10) . ? C20 Cl3 1.761(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N14 93.0(3) . . ? C1 Pd N12 171.0(3) . . ? N14 Pd N12 78.6(2) . . ? C1 Pd Cl 87.2(2) . . ? N14 Pd Cl 175.22(14) . . ? N12 Pd Cl 101.39(15) . . ? C2 Fe C3 41.0(3) . . ? C2 Fe C7 106.7(2) . . ? C3 Fe C7 124.7(3) . . ? C2 Fe C11 115.8(3) . . ? C3 Fe C11 103.9(3) . . ? C7 Fe C11 40.7(3) . . ? C2 Fe C10 151.8(4) . . ? C3 Fe C10 117.7(4) . . ? C7 Fe C10 68.2(3) . . ? C11 Fe C10 41.9(4) . . ? C2 Fe C6 41.4(3) . . ? C3 Fe C6 69.8(3) . . ? C7 Fe C6 119.1(3) . . ? C11 Fe C6 151.5(3) . . ? C10 Fe C6 165.6(4) . . ? C2 Fe C4 68.5(2) . . ? C3 Fe C4 41.2(3) . . ? C7 Fe C4 163.1(4) . . ? C11 Fe C4 125.4(4) . . ? C10 Fe C4 107.9(3) . . ? C6 Fe C4 68.8(3) . . ? C2 Fe C9 165.8(4) . . ? C3 Fe C9 153.0(3) . . ? C7 Fe C9 67.4(3) . . ? C11 Fe C9 68.7(4) . . ? C10 Fe C9 39.7(4) . . ? C6 Fe C9 128.9(4) . . ? C4 Fe C9 120.9(3) . . ? C2 Fe C8 127.4(3) . . ? C3 Fe C8 163.4(3) . . ? C7 Fe C8 40.4(3) . . ? C11 Fe C8 68.8(3) . . ? C10 Fe C8 67.6(3) . . ? C6 Fe C8 109.1(3) . . ? C4 Fe C8 155.1(3) . . ? C9 Fe C8 39.9(3) . . ? C2 Fe C5 68.6(3) . . ? C3 Fe C5 69.0(3) . . ? C7 Fe C5 154.7(3) . . ? C11 Fe C5 164.3(3) . . ? C10 Fe C5 127.8(3) . . ? C6 Fe C5 40.8(3) . . ? C4 Fe C5 40.4(4) . . ? C9 Fe C5 110.9(3) . . ? C8 Fe C5 121.7(3) . . ? C3 C2 N12 127.2(6) . . ? C3 C2 C6 109.3(6) . . ? N12 C2 C6 123.5(6) . . ? C3 C2 Fe 70.0(4) . . ? N12 C2 Fe 125.7(4) . . ? C6 C2 Fe 69.9(3) . . ? C2 C3 C4 106.7(7) . . ? C2 C3 Fe 69.0(4) . . ? C4 C3 Fe 69.7(4) . . ? C5 C4 C3 108.9(6) . . ? C5 C4 Fe 70.4(4) . . ? C3 C4 Fe 69.1(4) . . ? C4 C5 C6 108.3(7) . . ? C4 C5 Fe 69.2(4) . . ? C6 C5 Fe 68.8(4) . . ? C5 C6 C2 106.7(7) . . ? C5 C6 Fe 70.3(4) . . ? C2 C6 Fe 68.7(3) . . ? C8 C7 C11 109.6(6) . . ? C8 C7 Fe 70.3(4) . . ? C11 C7 Fe 69.7(4) . . ? C9 C8 C7 107.6(8) . . ? C9 C8 Fe 70.0(5) . . ? C7 C8 Fe 69.3(4) . . ? C10 C9 C8 109.3(7) . . ? C10 C9 Fe 69.8(5) . . ? C8 C9 Fe 70.1(4) . . ? C9 C10 C11 108.3(7) . . ? C9 C10 Fe 70.5(4) . . ? C11 C10 Fe 69.0(4) . . ? C7 C11 C10 105.3(8) . . ? C7 C11 Fe 69.6(4) . . ? C10 C11 Fe 69.1(4) . . ? C12 N12 C2 116.1(5) . . ? C12 N12 Pd 110.9(4) . . ? C2 N12 Pd 132.9(4) . . ? N12 C12 C13 119.2(6) . . ? N14 C13 C18 121.9(6) . . ? N14 C13 C12 116.9(6) . . ? C18 C13 C12 121.1(6) . . ? C15 N14 C13 117.2(6) . . ? C15 N14 Pd 128.6(5) . . ? C13 N14 Pd 114.0(4) . . ? N14 C15 C16 122.9(7) . . ? C17 C16 C15 120.1(6) . . ? C16 C17 C18 118.9(7) . . ? C17 C18 C13 118.9(7) . . ? C1' Pd' N14' 91.8(3) . . ? C1' Pd' N12' 170.7(3) . . ? N14' Pd' N12' 79.1(2) . . ? C1' Pd' Cl' 87.4(3) . . ? N14' Pd' Cl' 179.0(2) . . ? N12' Pd' Cl' 101.68(13) . . ? C2' Fe' C6' 41.2(3) . . ? C2' Fe' C10' 159.1(3) . . ? C6' Fe' C10' 158.7(3) . . ? C2' Fe' C8' 122.4(3) . . ? C6' Fe' C8' 106.6(3) . . ? C10' Fe' C8' 68.1(3) . . ? C2' Fe' C3' 41.6(2) . . ? C6' Fe' C3' 69.4(3) . . ? C10' Fe' C3' 122.7(3) . . ? C8' Fe' C3' 159.7(3) . . ? C2' Fe' C4' 69.0(3) . . ? C6' Fe' C4' 68.7(3) . . ? C10' Fe' C4' 108.1(3) . . ? C8' Fe' C4' 158.1(3) . . ? C3' Fe' C4' 40.7(3) . . ? C2' Fe' C9' 158.4(3) . . ? C6' Fe' C9' 122.1(3) . . ? C10' Fe' C9' 40.7(3) . . ? C8' Fe' C9' 40.3(3) . . ? C3' Fe' C9' 158.6(3) . . ? C4' Fe' C9' 122.7(3) . . ? C2' Fe' C5' 68.6(3) . . ? C6' Fe' C5' 40.3(3) . . ? C10' Fe' C5' 123.6(3) . . ? C8' Fe' C5' 121.9(3) . . ? C3' Fe' C5' 68.6(3) . . ? C4' Fe' C5' 40.8(3) . . ? C9' Fe' C5' 107.4(3) . . ? C2' Fe' C7' 107.0(3) . . ? C6' Fe' C7' 121.8(3) . . ? C10' Fe' C7' 68.4(3) . . ? C8' Fe' C7' 40.4(3) . . ? C3' Fe' C7' 123.7(2) . . ? C4' Fe' C7' 160.3(3) . . ? C9' Fe' C7' 68.1(3) . . ? C5' Fe' C7' 157.4(3) . . ? C2' Fe' C11' 122.3(3) . . ? C6' Fe' C11' 158.2(3) . . ? C10' Fe' C11' 41.1(3) . . ? C8' Fe' C11' 68.3(3) . . ? C3' Fe' C11' 107.7(3) . . ? C4' Fe' C11' 124.0(3) . . ? C9' Fe' C11' 68.6(3) . . ? C5' Fe' C11' 160.5(3) . . ? C7' Fe' C11' 40.6(3) . . ? N12' C2' C6' 125.0(5) . . ? N12' C2' C3' 127.5(5) . . ? C6' C2' C3' 107.5(5) . . ? N12' C2' Fe' 125.4(4) . . ? C6' C2' Fe' 69.5(4) . . ? C3' C2' Fe' 69.6(3) . . ? C4' C3' C2' 107.3(6) . . ? C4' C3' Fe' 69.7(4) . . ? C2' C3' Fe' 68.8(3) . . ? C3' C4' C5' 108.3(6) . . ? C3' C4' Fe' 69.7(4) . . ? C5' C4' Fe' 69.8(4) . . ? C6' C5' C4' 108.7(6) . . ? C6' C5' Fe' 69.4(4) . . ? C4' C5' Fe' 69.4(4) . . ? C5' C6' C2' 108.2(6) . . ? C5' C6' Fe' 70.3(4) . . ? C2' C6' Fe' 69.3(3) . . ? C8' C7' C11' 108.5(6) . . ? C8' C7' Fe' 69.5(4) . . ? C11' C7' Fe' 70.4(4) . . ? C9' C8' C7' 108.8(7) . . ? C9' C8' Fe' 70.1(4) . . ? C7' C8' Fe' 70.1(4) . . ? C8' C9' C10' 107.8(6) . . ? C8' C9' Fe' 69.6(4) . . ? C10' C9' Fe' 69.4(4) . . ? C9' C10' C11' 108.4(7) . . ? C9' C10' Fe' 70.0(4) . . ? C11' C10' Fe' 70.6(4) . . ? C7' C11' C10' 106.4(6) . . ? C7' C11' Fe' 69.0(4) . . ? C10' C11' Fe' 68.3(4) . . ? C12' N12' C2' 116.9(5) . . ? C12' N12' Pd' 109.5(4) . . ? C2' N12' Pd' 133.5(4) . . ? N12' C12' C13' 120.3(6) . . ? N14' C13' C18' 122.7(6) . . ? N14' C13' C12' 116.8(5) . . ? C18' C13' C12' 120.5(6) . . ? C15' N14' C13' 118.4(6) . . ? C15' N14' Pd' 127.7(5) . . ? C13' N14' Pd' 114.0(4) . . ? N14' C15' C16' 121.3(7) . . ? C17' C16' C15' 120.0(7) . . ? C16' C17' C18' 118.9(7) . . ? C13' C18' C17' 118.6(7) . . ? Cl2 C20 Cl3 109.2(5) . . ? _refine_diff_density_max 0.682 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.099